CN106245149A - A kind of high uniformity car mould polyester industrial fiber and preparation method thereof - Google Patents
A kind of high uniformity car mould polyester industrial fiber and preparation method thereof Download PDFInfo
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- CN106245149A CN106245149A CN201610778068.1A CN201610778068A CN106245149A CN 106245149 A CN106245149 A CN 106245149A CN 201610778068 A CN201610778068 A CN 201610778068A CN 106245149 A CN106245149 A CN 106245149A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- 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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D4/00—Spinnerette packs; Cleaning thereof
- D01D4/02—Spinnerettes
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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
- D01D5/08—Melt spinning methods
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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)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Polyesters Or Polycarbonates (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to a kind of high uniformity car mould polyester industrial fiber and preparation method thereof, the raw material of high uniformity car mould polyester industrial fiber is the modified poly ester being made up of p-phthalic acid segment, ethylene glycol segment and the dihydroxylic alcohols segment containing side chain.The preparation method of high uniformity car mould polyester industrial fiber is by p-phthalic acid and the dihydroxylic alcohols containing side chain, in the catalysis of concentrated sulphuric acid, carries out esterification and obtains phthalic acid binary alcohol esters；Then phthalic acid and ethylene glycol are made into and carry out esterification, obtain ethylene glycol terephthalate；Finally both are stirred mixing, under the effect of catalyst and stabilizer, carry out the polycondensation reaction of coarse vacuum stage and high vacuum stage of Fig, prepare modified poly ester, modified poly ester extrude through metering, porous spinneret, cool down, oils, is stretched, thermal finalization and winding, prepared high uniformity car mould polyester industrial fiber.
Description
Technical field
The invention belongs to polyester fiber technical field, relate to a kind of high uniformity car mould polyester industrial fiber and preparation method thereof.
Background technology
Polyethylene terephthalate (PET or polyester fiber) fiber from come out since, have fracture strength and
Elastic modelling quantity is high, and resilience is moderate, and thermal finalization is excellent, and heat-resisting light resistance is good and acid-fast alkali-proof corrosion resistance etc. is a series of excellent
Performance, and fabric have crease-resistant exempt from money, the advantages such as stiffness is good, be widely used in the field such as clothing, home textile.
Pet Industrial Fiber is primarily referred to as mostly being applied to industry, national defence, medical treatment, environmental conservation and most advanced branches of science each side
Face, is to have the most special physicalchemical structure, performance and purposes, or has the chemical fibre of specific function, major embodiment
Being able to bear strong corrosion, low abrasion, high temperature resistant, radiation hardness, fire-retardant, fire-resistant, high voltage withstanding, high strength and modulus and plurality of medical merit
Energy.Using high-strength low-shrinkage polyester industrial filament yarn as the PVC shelter cloth of raw material production, there is higher peel strength and tear is strong
Degree, makes shelter cloth be applicable to various uses, flexible body advertising lamp box material, inflatable structure material, fluffy lid architectural fabrics sunshade account
Paulin etc..It is that main textile material obtains in terms of the military supplies such as special protective garment, camouflage, covering, knapsack with high-strength low-shrinkage industrial yarn
To application.One as earth working material has the advantages such as light, soft, high-strength, wear-resisting, anticorrosive, non-conductive, damping.Make
Used time safe ready, efficiency are high, and will not damage lifting object.The application of Pet Industrial Fiber is expanded and is driven application
The whole competitiveness in field promotes, and no matter is alleviating the weight of composite, and the durability of use and minimizing are keeped in repair, raised cost
Etc. all many-sides, polyesters high-performance fiber has increasingly given play to its synthetic competitive advantages.Following many decades, high-performance polyester
The development of fiber has considerable progress the most in quantity, more in the expansion of application and carrying of industrial chain whole competitiveness
Go up the substantial effect of acquirement.
High uniformity and functionalization will be the Main way of Pet Industrial Fiber development, and affect fiber quality is poly-
Ester high molecular collection state structure, the active force being mainly concerned with between polyester molecule, the form of crystallization and structure, orientation structure
Deng, and the form crystallized and structure are emphasis therein.
Have many parameters during melt spinning, these parameters determine fiberizing course and spin fiber structure and
Performance, production is through the fiber controlling these parameters to prepare desired properties.Experimental branch line all uses side for a long time
Blowing is as the type of cooling, and energy resource consumption accounts for the significant portion of long filament production cost, along with people are to chemical fibre performance and quality
Requiring day by day to improve, the exploitation of chemical-fibres filaments new product develops to the fibre in differentiation direction of high added value, it is desirable to higher cold
But dry condition, then propose ring blowing device.Ring blowing device not only possesses every uniform advantage of synnema wind-engaging, Er Qieneng
Consumption is compared relatively low, effectively solves the wind energy loss problem that cross air blasting causes owing to blowing area is big.
In spinning process, although ring blowing has obvious advantage, but still the cooling of porous yarn cannot be solved well
Uneven problem: owing to spun silk is after circular jetting filament plate is extruded, by ring quenching, due to the circular jetting filament plate number of turns relatively
It is many so that ring blowing hardly enters innermost layer, causes the silk at outermost silk innermost layer the most after cooling may be the most uncolled,
Thus the problem such as the silk of gained occurs that fiber number is irregular, and intensity is irregular, cause and follow-up silk is processed further difficulty occur.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, it is provided that a kind of high uniformity car mould polyester work
Industry silk and preparation method thereof, the raw material of high uniformity car mould polyester industrial fiber of the present invention is modified poly ester, the molecule of modified poly ester
Chain introduces the dihydroxylic alcohols segment containing side chain, is modified modified high uniformity car mould polyester industrial fiber prepared by polyester, a constant temperature
Under the conditions of degree, the increasing degree of the spatial joint clearance of high uniformity car mould polyester industrial fiber interior molecules interchain is far longer than same isothermal
Unbranched high uniformity car mould polyester industrial fiber under degree, the melt viscosity of high uniformity car mould polyester industrial fiber reduces, and reduces
Processing temperature, reduces degradation rate, is conducive to processing.The additionally porous spray webbing of the high uniformity car mould polyester industrial fiber of the present invention
On plate, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refers to that the hole of spinneret orifice is centrally located on concentration ellipse,
Concentration ellipse is that series is oval, the major axis conllinear of all ellipses, and short axle conllinear；Higher cooling effectiveness and preferably can be reached
Cooling effect.
A kind of high uniformity car mould polyester industrial fiber, described high uniformity car mould polyester industrial fiber by modified poly ester through solid phase
After thickening, spinning obtains；The material of described high uniformity car mould polyester industrial fiber is modified poly ester, and described modified poly ester is by benzene two
Formic acid segment, ethylene glycol segment and the composition of the dihydroxylic alcohols segment containing side chain, the described dihydroxylic alcohols segment containing side chain refers to side chain position
On a non-end group carbon in dihydroxylic alcohols segment and dihydroxylic alcohols segment that side chain is the linear carbon chain containing 5-10 carbon atom；
Described high uniformity car mould polyester industrial fiber is at 260～290 DEG C, and melt viscosity declines 10-20%, temperature be 177 DEG C ×
Under the test condition of 10min × 0.05cN/dtex, dry-hot shrinkage is 7.0 ± 0.5%；Described high uniformity car mould polyester work
The fracture strength of industry silk >=7.7cN/dtex line density deviation ratio≤1.0%, fracture strength CV value≤2.0%, extension at break CV
Value≤5.5%.
Described melt viscosity declines the contrast referring to modified poly ester and normal polyester in mutually synthermal melt viscosity.
A kind of high uniformity car mould polyester industrial fiber is modified poly ester, introduces containing side chain on modified poly ester macromole long-chain
Dihydroxylic alcohols segment, and the length of side chain and quantity are relatively big on the crystal property of modified poly ester and the impact of flow behavior, side chain
The shortest purpose not reaching polyester modification of length, the oversize meeting of length causes new entanglement, affects its flow behavior, when side chain is positioned at
On a non-end group carbon in dihydroxylic alcohols segment and when side chain is the linear carbon chain containing 5-10 carbon atom, it is modified polyester system
Standby a kind of high uniformity car mould polyester industrial fiber, under the conditions of uniform temperature, the spatial joint clearance of industrial yarn interior molecules interchain
Increasing degree be far longer than unbranched industrial yarn at equal temperature, beneficially industrial yarn melt viscosity reduces, it is simple to enter one
The processing of step.
As preferred technical scheme:
A kind of high uniformity car mould polyester industrial fiber as above, the fracture of described high uniformity car mould polyester industrial fiber
Elongation 19.0 ± 1.5%；The number-average molecular weight of described modified poly ester is 15000-30000.
High uniformity car mould polyester industrial fiber as above a kind of, the described dihydroxylic alcohols segment containing side chain be 2-amyl group-
1,3 propylene glycol segments, 2-hexyl-1,3 propylene glycol segment, 2-heptyl-1,3 propylene glycol segment, 2-octyl group-1,3 propylene glycol segment,
2-nonyl-1,3 propylene glycol segment, 2-decyl-1,3 propylene glycol segment, 2-amyl group-1,4 butanediol segment, 2-hexyl-1,4 fourth two
Alcohol segment, 2-heptyl-1,4 butanediol segment, 2-octyl group-1,4 butanediol segment, 2-nonyl-1,4 butanediol segment, 2-decyl-
1,4 butanediol segments, 2-amyl group-1,5 pentanediol segment, 2-hexyl-1,5 pentanediol segment, 2-heptyl-1,5 pentanediol segment,
2-octyl group-1,5 pentanediol segment, 2-nonyl-1,5 pentanediol segment, 2-decyl-1,5 pentanediol segment, 2-amyl group-1,6 oneself two
Alcohol segment, 2-hexyl-1,6 hexanediol segment, 2-heptyl-1,6 hexanediol segment, 2-octyl group-1,6 hexanediol segment, 2-nonyl-
More than one in 1,6 hexanediol segments or 2-decyl-1,6 hexanediol segment；The described dihydroxylic alcohols segment containing side chain and second two
The Mole percent ratio of alcohol segment is 2～5%.
The preparation method of a kind of high uniformity car mould polyester industrial fiber of the present invention, increases modified poly ester through solid phase polycondensation
Viscous, metering, porous spinneret extrudes, cool down, oil, are stretched, thermal finalization and winding, prepared high uniformity car mould polyester industrial
Silk；
On described porous spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, and described oval shaped arrangements refers to spinneret orifice
Hole be centrally located on concentration ellipse, described concentration ellipse is that series is oval, the major axis conllinear of all ellipses, and short axle conllinear；
The preparation process of modified poly ester comprises the following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
After p-phthalic acid is made into slurry with the dihydroxylic alcohols containing side chain, under the catalytic action of concentrated sulphuric acid, it is esterified
Reaction, obtains p-phthalic acid binary alcohol esters；The described dihydroxylic alcohols containing side chain is that be positioned in dihydroxylic alcohols segment one of side chain is non-
On end group carbon and dihydroxylic alcohols that side chain is the linear carbon chain containing 5-10 carbon atom；
For the dihydroxylic alcohols containing side chain, its side chain is alkyl, is electron withdraw group, in the existence of side chain, makes strand
Spatial volume increases, and solvation diminishes, and in dihydroxylic alcohols, proton is difficult to dissociation so that the dihydroxylic alcohols containing side chain and terephthaldehyde
The reactivity of acid, less than ethylene glycol, according to the mixing of same ethylene glycol and terephthaldehyde's acid reaction, can cause the binary containing side chain
Alcohol reaction is imperfect, thus the ratio that the dihydroxylic alcohols that impact is containing side chain is in polyester macromolecule, and then affect the performance of polyester.This
Invention uses and first with p-phthalic acid, the dihydroxylic alcohols containing side chain is carried out esterification under the catalytic action of sulphuric acid, and its product exists
Ethylene glycol and p phthalic acid esterification add after terminating, it is ensured that the stability of the dihydroxylic alcohols proportioning containing side chain.
(2) preparation of ethylene glycol terephthalate:
After p-phthalic acid and ethylene glycol are made into slurry, carry out esterification, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), stir
Mix mixing, under the effect 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, prepares modified poly ester.
The preparation method of a kind of high uniformity car mould polyester industrial fiber as above, prepared by described modified poly ester concrete
Step is:
(1) preparation of p-phthalic acid binary alcohol esters:
P-phthalic acid and the dihydroxylic alcohols containing side chain are made into slurry and add in reactor, in the catalytic action of concentrated sulphuric acid
Under, carrying out esterification, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is normal pressure～0.3MPa, and temperature is 180
～240 DEG C, it is esterification terminal when the water quantity of distillate in esterification reaches more than the 90% of theoretical value；Obtain benzene two
Formic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate:
Adding in reactor after p-phthalic acid and ethylene glycol are made into slurry, carry out esterification, esterification is at nitrogen
Atmosphere encloses middle compressive reaction, and moulding pressure is normal pressure～0.3MPa, and temperature is 250～260 DEG C, when the water in esterification distillates
Amount reach theoretical value more than 90% time be esterification terminal, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), stir
Mixing mixing 15-20 minute, under the effect 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 temperature controls at 260～270 DEG C, and the response time is
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, response time 50～90 minutes, prepares modified poly ester；
Again through pelletizing, modified poly ester being obtained Modified polyester chips, obtained polyester slice is viscosified by solid phase polycondensation, makes
The intrinsic viscosity of polyester slice brings up to 1.0～1.2dL/g, is high viscous section；Again through metering, porous spinneret extrusion, cold
But, oil, stretch, thermal finalization and winding, prepare high uniformity car mould polyester industrial fiber；
Spinning main technologic parameters is:
The temperature of described extrusion is 290～320 DEG C；
The pathogenic wind-warm of described cooling is 20～30 DEG C；
The described oil applying rate oiled is 0.4～0.8wt%；
The speed of described winding is 2600～3400m/min.
The preparation method of a kind of high uniformity car mould polyester industrial fiber as above, in described step (1), terephthaldehyde
Acid is 1:1.3-1.5 with the mol ratio of the dihydroxylic alcohols containing side chain；Concentrated sulphuric acid addition is the 0.3-of p-phthalic acid weight
0.5%；The concentration of described concentrated sulphuric acid is 50-60wt%；In described step (2), p-phthalic acid with the mol ratio of ethylene glycol is
1:1.2～2.0；In described step (3), described p-phthalic acid binary alcohol esters and the Mole percent of ethylene glycol terephthalate
Ratio is 2～5%；Described catalyst is antimony oxide, antimony glycol or antimony acetate, and catalyst charge is p-phthalic acid
The 0.01%～0.05% of gross weight；Described stabilizer is triphenyl phosphate, trimethyl phosphate or NSC 6513, stabilizer
Addition is the 0.01%～0.05% of described p-phthalic acid gross weight.
The preparation method of a kind of high uniformity car mould polyester industrial fiber as above, the described dihydroxylic alcohols containing side chain is 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, 2-decyl-1,3 propylene glycol, 2-amyl group-1,4 butanediol, 2-hexyl-1,4 butanediol, 2-heptyl-1,4 butanediol, 2-
Octyl group-1,4 butanediol, 2-nonyl-1,4 butanediol, 2-decyl-1,4 butanediol, 2-amyl group-1,5 pentanediol, 2-hexyl-1,5
Pentanediol, 2-heptyl-1,5 pentanediol, 2-octyl group-1,5 pentanediol, 2-nonyl-1,5 pentanediol, 2-decyl-1,5 pentanediol, 2-
Amyl group-1,6 hexanediol, 2-hexyl-1,6 hexanediol, 2-heptyl-1,6 hexanediol, 2-octyl group-1,6 hexanediol, 2-nonyl-1,6
More than one in hexanediol or 2-decyl-1,6 hexanediol.
The preparation method of a kind of high uniformity car mould polyester industrial fiber as above, described porous spinneret is circular jetting
Filament plate or elliptical spinneret plate；The difference of the long axis length that the diameter of described circular jetting filament plate is maximum with series ellipse is more than
10mm, the difference of the long axis length that described elliptical spinneret plate is maximum with series ellipse is more than 10mm.
The preparation method of a kind of high uniformity car mould polyester industrial fiber as above, spinneret orifice on described porous spinneret
Be arranged as major axis and/or short axial symmetry, the spacing of adjacent spinneret orifice more than or equal to the guide hole diameter of spinneret orifice plus 1.5mm；
Oval major axis is 1.3～1.8 with the ratio of minor axis length.
When the effective area phase of spinneret is simultaneously as the girth of ellipse is more than circular girth, and 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, therefore, and spray
Silk hole oval shaped arrangements is conducive to the cooling that ring is dried, and improves the cooling effectiveness of ring blowing, and the fibre property of preparation is the most excellent
Good.Major axis is closer to 1 with the ratio of minor axis length, and ellipse is more similar to circle, and the difference of cooling effectiveness and cooling effect is little；
When the ratio of major axis and minor axis length is 1.3, cooling effect significantly improves, and individual pen hole count increases by 16% accordingly；Major axis and short axle
When the ratio of length is 1.8, cooling effect improves relatively big, and individual pen hole count increases by 33%, in the case of identical hole count, the present invention accordingly
Oval shaped arrangements reduce than the number of turns of conventional concentric circle best-fit, it is easy to cooling wind is saturating, makes the fiber cooling condition of Internal and external cycle
Evenly；When the ratio of major axis and minor axis length is more than 1.8, ellipse is partial to form flat shape, is difficult to punching, the coldest
But effect no longer raises.Therefore, the major axis that series is oval is 1.3～1.8 with the ratio of minor axis length, it is possible to reach higher cold
But efficiency and preferable cooling effect.
The preparation method of a kind of high uniformity car mould polyester industrial fiber as above, the guide hole of described spinneret orifice is a diameter of
1.5～2.5mm；The spray webbing hole count of described spinneret is more than or equal to 192, and the shape of cross section of the spinneret orifice of described spinneret is
Circle, square, rhombus, yi word pattern, triangular form, trilobal cross, hollow type or platypelloid type.
The principle of the present invention is:
The raw material of the high uniformity car mould polyester industrial fiber of the present invention is modified poly ester, contains in modified poly ester macromole
Dihydroxylic alcohols 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, the free volume being modified industrial yarn prepared by polyester is far longer than unbranched industrial yarn at equal temperature, favorably
In reducing its melt viscosity.
On the spinneret of the present invention, the arrangement mode of spinneret orifice is oval shaped arrangements, when the effective area of spinneret is identical,
The number of plies of spinneret orifice oval shaped arrangements is easier to blow through dynamic analysis of spinning less than the number of plies of circular arrangement, ring blowing, dynamic analysis of spinning
Cooling effect is more preferable, and the industrial yarn of preparation is the most more excellent.When the effective area of spinneret is identical, spinneret orifice oval shaped arrangements
Hole count is more than the hole count of circular arrangement, and oval shaped arrangements is capable of cooling down greatly, significantly improves cooling effectiveness.
Beneficial effect:
The raw material of the high uniformity car mould polyester industrial fiber of gained of the present invention is modified poly ester, contains in modified poly ester macromole
The dihydroxylic alcohols segment containing side chain having, when temperature is higher than vitrification point, side chain, prior to backbone motion, makes the increasing of free volume
Adding amplitude and be far longer than the characteristic of unbranched polyester macromolecule chain, the increase of free volume advantageously reduces melt viscosity, changes
Its processing characteristics kind.
The raw material of the high uniformity car mould polyester industrial fiber of gained of the present invention is modified poly ester, the dihydroxylic alcohols segment containing side chain
Introduce to the structural regularity of modified poly ester there is no big destruction, maintain the premium properties of polyester fiber.
On the high uniformity car mould polyester industrial fiber spinneret of the present invention, the arrangement mode of spinneret orifice is oval shaped arrangements, spray
When the effective area of filament plate is identical, the number of plies of spinneret orifice oval shaped arrangements is easier to blow less than the number of plies of circular arrangement, ring blowing
Dynamic analysis of spinning thoroughly, the cooling effect of dynamic analysis of spinning is more preferable, and the fibre property of preparation is the most more excellent.
On the high uniformity car mould polyester industrial fiber spinneret of the present invention, the arrangement mode of spinneret orifice is oval shaped arrangements, spray
When the effective area of filament plate is identical, the hole count of spinneret orifice oval shaped arrangements is more than the hole count of circular arrangement, and oval shaped arrangements can
Realize cooling down greatly, significantly improve cooling effectiveness.
Accompanying drawing explanation
Fig. 1 is the oval shaped arrangements figure of 374 spinneret orifices, and the aperture of spinneret orifice is 2.0mm, transverse and the length of 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, transverse and the length of short axle
Degree ratio is 1.6.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate this
Bright rather than limit the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, art technology
The present invention can be made various changes or modifications by personnel, and these equivalent form of values fall within the application appended claims equally and limited
Fixed scope.
Embodiment 1
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.3 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 the concentrated sulphuric acid of the 0.3% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is normal pressure, and temperature is 180 DEG C, when the water in esterification distillates
Amount reach theoretical value 90% time be esterification terminal, obtain p-phthalic acid binary alcohol esters；
(2) preparation of ethylene glycol terephthalate:
Mol ratio is 1:1.2 p-phthalic acid and ethylene glycol be made into slurry after add in reactor, carry out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is normal pressure, and temperature is 250 DEG C, when the water in esterification distillates
Amount reach theoretical value 90% time be esterification terminal, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 2% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 15 minutes, is adding
The catalytic antimony trioxide and addition that amount is the 0.01% of p-phthalic acid gross weight are p-phthalic acid gross weight
Under the effect of the stabilizer triphenyl phosphate of 0.01%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
It is 500Pa that section pressure is steadily evacuated to absolute pressure by normal pressure, and temperature controls at 260 DEG C, and the response time is 30 minutes；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 100Pa, and reaction temperature controls
275 DEG C, in 50 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 15000, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2-penta
Base-1,3 propylene glycol segment compositions, the dihydroxylic alcohols segment containing side chain is 2% with the Mole percent ratio of ethylene glycol segment.
Table 1: embodiment 2-12 important technological parameters
Embodiment 2
The preparation method of the modified poly ester of embodiment 2, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 16 minutes, in addition be
The catalytic antimony trioxide of the 0.011% of p-phthalic acid gross weight and addition is p-phthalic acid gross weight 0.02%
Stabilizer triphenyl phosphate effect under, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure
Steadily be evacuated to absolute pressure 490Pa by normal pressure, temperature controls at 262 DEG C, and the response time is 31 minutes；Then proceed to evacuation,
Carrying out the polycondensation reaction of high vacuum stage of Fig, make reaction pressure be down to absolute pressure 90Pa, reaction temperature controls at 276 DEG C, reaction
51 minutes time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 16000, and modified poly ester is own by p-phthalic acid segment, ethylene glycol segment and 2-
Base-1,3 propylene glycol segment compositions, 2-hexyl-1,3 propylene glycol segments are 2.1% with the Mole percent ratio of ethylene glycol segment.
Embodiment 3
The preparation method of the modified poly ester of embodiment 3, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 16 minutes, in addition be
The catalytic antimony trioxide of the 0.03% of p-phthalic acid gross weight and addition is p-phthalic acid gross weight 0.02%
Stabilizer triphenyl phosphate effect under, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure
Steadily be evacuated to absolute pressure 498Pa by normal pressure, temperature controls at 263 DEG C, and the response time is 32 minutes；Then proceed to evacuation,
Carrying out the polycondensation reaction of high vacuum stage of Fig, make reaction pressure be down to absolute pressure 90Pa, reaction temperature controls at 277 DEG C, reaction
57 minutes time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 15900, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2-heptan
Base-1,3 propylene glycol segment compositions, 2-heptyl-1,3 propylene glycol segments are 2.2% with the Mole percent ratio of ethylene glycol segment.
Embodiment 4
The preparation method of the modified poly ester of embodiment 4, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 17 minutes, in addition be
The catalytic antimony trioxide of the 0.033% of p-phthalic acid gross weight and addition are p-phthalic acid gross weight
Under the effect of the stabilizer triphenyl phosphate of 0.023%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
It is 497Pa that section pressure is steadily evacuated to absolute pressure by normal pressure, and temperature controls at 264 DEG C, and the response time is 33 minutes；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, in 58 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 15800, and modified poly ester is pungent by p-phthalic acid segment, ethylene glycol segment and 2-
Base-1,3 propylene glycol segment compositions, 2-octyl group-1,3 propylene glycol segments are 2.3% with the Mole percent ratio of ethylene glycol segment.
Embodiment 5
The preparation method of the modified poly ester of embodiment 5, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 17 minutes, in addition be
The catalytic antimony trioxide of the 0.034% of p-phthalic acid gross weight and addition are p-phthalic acid gross weight
Under the effect of the stabilizer triphenyl phosphate of 0.024%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
Section pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature controls at 265 DEG C, and the response time is 34 minutes；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 80Pa, and reaction temperature controls 277
DEG C, in 59 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 15900, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2-nonyl
Base-1,3 propylene glycol segment compositions, 2-nonyl-1,3 propylene glycol segments are 2.4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 6
The preparation method of the modified poly ester of embodiment 6, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 18 minutes, in addition be
The catalytic antimony trioxide of the 0.035% of p-phthalic acid gross weight and addition are p-phthalic acid gross weight
Under the effect of the stabilizer triphenyl phosphate of 0.025%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
Section pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and temperature controls at 266 DEG C, and the response time is 35 minutes；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, in 60 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 16000, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2-last of the ten Heavenly stems
Base-1,3 propylene glycol segment compositions, 2-decyl-1,3 propylene glycol segments are 2.5% with the Mole percent ratio of ethylene glycol segment.
Embodiment 7
The preparation method of the modified poly ester of embodiment 7, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 19 minutes, in addition be
The catalytic antimony trioxide of the 0.036% of p-phthalic acid gross weight and addition are p-phthalic acid gross weight
Under the effect of the stabilizer triphenyl phosphate of 0.025%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
Section pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature controls at 267 DEG C, and the response time is 36 minutes；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, in 61 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 16000, and the number-average molecular weight of modified poly ester is 16000, and modified poly ester is by right
Phthalic acid segment, ethylene glycol segment and 2-amyl group-Isosorbide-5-Nitrae butanediol segment composition, 2-amyl group-Isosorbide-5-Nitrae butanediol segment and second two
The Mole percent ratio of alcohol segment is 2.6%.
Embodiment 8
The preparation method of the modified poly ester of embodiment 8, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 19 minutes, in addition be
The catalytic antimony trioxide of the 0.036% of p-phthalic acid gross weight and addition are p-phthalic acid gross weight
Under the effect of the stabilizer triphenyl phosphate of 0.025%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
Section pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature controls at 267 DEG C, and the response time is 36 minutes；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, in 61 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 17000, and modified poly ester is own by p-phthalic acid segment, ethylene glycol segment and 2-
Base-Isosorbide-5-Nitrae butanediol segment composition, 2-hexyl-Isosorbide-5-Nitrae butanediol segment is 2.7% with the Mole percent ratio of ethylene glycol segment.
Embodiment 9
The preparation method of the modified poly ester of embodiment 9, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 16 minutes, in addition be
The catalyst glycol antimony of the 0.04% of p-phthalic acid gross weight and addition is p-phthalic acid gross weight 0.026%
Under the effect 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 temperature controls at 268 DEG C, and the response time is 38 minutes；Then proceed to evacuation, enter
The polycondensation reaction of row high vacuum stage of Fig, making reaction pressure be down to absolute pressure is 60Pa, and reaction temperature controls at 279 DEG C, reaction
62 minutes time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 17000, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2-heptan
Base-Isosorbide-5-Nitrae butanediol segment composition, 2-heptyl-Isosorbide-5-Nitrae butanediol segment is 2.8% with the Mole percent ratio of ethylene glycol segment.
Embodiment 10
The preparation method of the modified poly ester of embodiment 10, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 17 minutes, in addition be
The catalyst glycol antimony of the 0.03% of p-phthalic acid gross weight and addition is p-phthalic acid gross weight 0.027%
Under the effect 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 temperature controls at 269 DEG C, and the response time is 39 minutes；Then proceed to evacuation, enter
The polycondensation reaction of row high vacuum stage of Fig, making reaction pressure be down to absolute pressure is 60Pa, and reaction temperature controls at 278 DEG C, reaction
64 minutes time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 17000, and modified poly ester is pungent by p-phthalic acid segment, ethylene glycol segment and 2-
Base-Isosorbide-5-Nitrae butanediol segment composition, 2-octyl group-Isosorbide-5-Nitrae butanediol segment is 3% with the Mole percent ratio of ethylene glycol segment.
Embodiment 11
The preparation method of the modified poly ester of embodiment 11, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 18 minutes, in addition be
The catalyst glycol antimony of the 0.04% of p-phthalic acid gross weight and addition is p-phthalic acid gross weight 0.03%
Under the effect 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 temperature controls at 260 DEG C, and the response time is 40 minutes；Then proceed to evacuation, enter
The polycondensation reaction of row high vacuum stage of Fig, making reaction pressure be down to absolute pressure is 60Pa, and reaction temperature controls at 277 DEG C, reaction
63 minutes time, prepare modified poly ester.
The number-average molecular weight of modified poly ester is 18000, and modified poly ester is by p-phthalic acid segment, ethylene glycol segment and 2-nonyl
Base-Isosorbide-5-Nitrae butanediol segment composition, 2-nonyl-Isosorbide-5-Nitrae butanediol segment is 4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 12
The preparation method of the modified poly ester of embodiment 12, wherein the preparation process of modified poly ester is with embodiment 1, mainly
Technical parameter see table 1；After step (3) adds p-phthalic acid binary alcohol esters, stirring mixing 18 minutes, in addition be
The catalyst acetic acid antimony of the 0.038% of p-phthalic acid weight and addition is p-phthalic acid weight 0.03% stabilizer
Under the effect of NSC 6513, starting the polycondensation reaction in coarse vacuum stage under conditions of negative pressure, this staged pressure is by normal pressure
Steadily being evacuated to absolute pressure 497Pa, temperature controls at 265 DEG C, and the response time is 42 minutes；Then proceed to evacuation, carry out height
The polycondensation reaction of vacuum stages, making reaction pressure be down to absolute pressure is 40Pa, and reaction temperature controls at 277 DEG C, the response time
70 minutes, prepare modified poly ester.
The number-average molecular weight of modified poly ester prepared is 26000, by p-phthalic acid segment, ethylene glycol segment and 2-last of the ten Heavenly stems
Base-Isosorbide-5-Nitrae butanediol segment composition, 2-decyl-Isosorbide-5-Nitrae butanediol segment is 4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 13
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.5 and 2-decyl-1,6 hexanediol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of the concentrated sulphuric acid of the 0.5% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.3MPa, and temperature is 240 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.3MPa, and temperature is 260 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 5% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 20 minutes, is adding
The catalyst acetic acid antimony of 0.05% that amount is p-phthalic acid weight and addition is p-phthalic acid weight 0.05% steady
Determine under the effect of 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 temperature controls at 270 DEG C, and the response time is 50 minutes；Then proceed to evacuation,
Carrying 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
Between Ying Shi 90 minutes, prepare modified poly ester.
The number-average molecular weight of modified poly ester prepared is 30000, by p-phthalic acid segment, ethylene glycol segment and 2-last of the ten Heavenly stems
Base-1,6 hexanediol segment compositions, 2-decyl-1,6 hexanediol segments are 5% with the Mole percent ratio of ethylene glycol segment.
Embodiment 14
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.47 and 2-nonyl-1,6 hexanediol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of the concentrated sulphuric acid of the 0.47% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 220 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.27MPa, and temperature is 258 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes, is adding
The catalyst glycol antimony of 0.04% that amount is p-phthalic acid weight and addition is p-phthalic acid weight 0.04%
Under the effect 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 temperature controls at 263 DEG C, and the response time is 47 minutes；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, prepare modified poly ester.
The number-average molecular weight of the modified poly ester prepared is 28000, by p-phthalic acid segment, ethylene glycol segment and 2-nonyl
Base-1,6 hexanediol segment compositions, 2-nonyl-1,6 hexanediol segments are 4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 15
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.46 and 2-octyl group-1,6 hexanediol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of the concentrated sulphuric acid of the 0.49% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 233 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 259 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.5% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 19 minutes, is adding
The catalytic antimony trioxide and the addition that enter amount is p-phthalic acid weight 0.044% are p-phthalic acid weight
Under the effect of the stabilizer triphenyl phosphate of 0.046%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
Section pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and temperature controls at 269 DEG C, and the response time is 48 minutes；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,
In 87 minutes response time, prepare modified poly ester.
The number-average molecular weight of the modified poly ester prepared is 29000, pungent by p-phthalic acid segment, ethylene glycol segment and 2-
Base-1,6 hexanediol segment compositions, 2-octyl group-1,6 hexanediol segments are 4.5% with the Mole percent ratio of ethylene glycol segment.
Embodiment 16
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.49 and 2-heptyl-1,6 hexanediol are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of the concentrated sulphuric acid of the 0.48% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 230 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 258 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.7% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 19 minutes, is adding
The catalyst glycol antimony and the addition that enter amount is p-phthalic acid weight 0.048% are p-phthalic acid weight
Under the effect of the stabilizer triphenyl phosphate of 0.047%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
Section pressure is steadily evacuated to absolute pressure 460Pa by normal pressure, and temperature controls at 267 DEG C, and the response time is 48 minutes；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,
In 83 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester prepared 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
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.467 and 2-hexyl-1,6 hexanediol are made into slurry and add in reactor,
Being 60wt% in concentration, addition is under the catalytic action of the concentrated sulphuric acid of the 0.47% of p-phthalic acid weight, carries out esterification anti-
Should, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.27MPa, and temperature is 236 DEG C, when in esterification
It is esterification terminal when water quantity of distillate reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification anti-
Should, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 258 DEG C, when in esterification
It is esterification terminal when water quantity of distillate reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.3% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes, is adding
The catalytic antimony trioxide and the addition that enter amount is p-phthalic acid weight 0.04% are p-phthalic acid weight
Under the effect of the stabilizer NSC 6513 of 0.041%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and temperature controls at 268 DEG C, and the response time is 48 minutes；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 40Pa, and reaction temperature controls 278
DEG C, in 85 minutes response time, prepare modified poly ester.
The number-average molecular weight of the modified poly ester prepared is 29000, own by p-phthalic acid segment, ethylene glycol segment and 2-
Base-1,6 hexanediol segment compositions, 2-hexyl-1,6 hexanediol segments are 4.3% with the Mole percent ratio of ethylene glycol segment.
Embodiment 18
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.48 and 2-amyl group-1,6 hexanediol are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of the concentrated sulphuric acid of the 0.46% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 230 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification anti-
Should, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 256 DEG C, when in esterification
It is esterification terminal when water quantity of distillate reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.7% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes, is adding
The catalytic antimony trioxide and the addition that enter amount is p-phthalic acid weight 0.047% are p-phthalic acid weight
Under the effect of the stabilizer triphenyl phosphate of 0.047%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
Section pressure is steadily evacuated to absolute pressure 480Pa by normal pressure, and temperature controls at 265 DEG C, and the response time is 47 minutes；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,
In 85 minutes response time, prepare modified poly ester.
The number-average molecular weight of the modified poly ester prepared is 28000, by p-phthalic acid segment, ethylene glycol segment and 2-penta
Base-1,6 hexanediol segment compositions, 2-amyl group-1,6 hexanediol segments are 4.7% with the Mole percent ratio of ethylene glycol segment.
Embodiment 19
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.46 and 2-decyl-1,5 pentanediols are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of the concentrated sulphuric acid of the 0.47% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 238 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 259 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches more than the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.7% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 19 minutes, is adding
Enter the catalyst acetic acid antimony of amount is p-phthalic acid weight 0.046% and addition is p-phthalic acid weight 0.048%
Stabilizer NSC 6513 effect under, 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 temperature controls at 267 DEG C, and the response time is 49 minutes；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,
In 87 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester prepared is 29000, by p-phthalic acid segment, ethylene glycol segment and 2-last of the ten Heavenly stems
Base-1,5 pentanediol segment compositions, 2-decyl-1,5 pentanediol segments are 4.7% with the Mole percent ratio of ethylene glycol segment.
Embodiment 20
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.46 and 2-nonyl-1,5 pentanediols are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of the concentrated sulphuric acid of the 0.46% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.26MPa, and temperature is 221 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification anti-
Should, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.25MPa, and temperature is 259 DEG C, when in esterification
It is esterification terminal when water quantity of distillate reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.1% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes, is adding
The catalyst glycol antimony and the addition that enter amount is p-phthalic acid weight 0.041% are p-phthalic acid weight
Under the effect of the stabilizer trimethyl phosphate of 0.042%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
Section pressure is steadily evacuated to absolute pressure 460Pa by normal pressure, and temperature controls at 265 DEG C, and the response time is 47 minutes；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,
In 85 minutes response time, prepare modified poly ester.
The number-average molecular weight of the modified poly ester prepared is 28000, by p-phthalic acid segment, ethylene glycol segment and 2-nonyl
Base-1,5 pentanediol segment compositions, 2-nonyl-1,5 pentanediol segments are 4.1% with the Mole percent ratio of ethylene glycol segment.
Embodiment 21
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.43 and 2-octyl group-1,5 pentanediols are made into slurry and add in reactor,
Concentration is 60wt%, and addition is under the catalytic action of the concentrated sulphuric acid of the 0.47% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.27MPa, and temperature is 235 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification anti-
Should, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.26MPa, and temperature is 255 DEG C, when in esterification
It is esterification terminal when water quantity of distillate reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.3% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 17 minutes, is adding
The catalytic antimony trioxide and the addition that enter amount is p-phthalic acid weight 0.043% are p-phthalic acid weight
Under the effect of the stabilizer triphenyl phosphate of 0.049%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
Section pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and temperature controls at 268 DEG C, and the response time is 46 minutes；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,
In 85 minutes response time, prepare modified poly ester.
The number-average molecular weight of the modified poly ester prepared is 28000, pungent by p-phthalic acid segment, ethylene glycol segment and 2-
Base-1,5 pentanediol segment compositions, 2-octyl group-1,5 pentanediol segments are 4.3% with the Mole percent ratio of ethylene glycol segment.
Embodiment 22
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.43 and 2-heptyl-1,5 pentanediols are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of the concentrated sulphuric acid of the 0.45% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.29MPa, and temperature is 235 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification anti-
Should, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.27MPa, and temperature is 255 DEG C, when in esterification
It is esterification terminal when water quantity of distillate reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.6% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes, is adding
Enter the catalyst glycol antimony of amount is p-phthalic acid weight 0.047% and addition is p-phthalic acid weight 0.04%
Stabilizer triphenyl phosphate effect under, under conditions of negative pressure start the coarse vacuum stage polycondensation reaction, this staged pressure
Steadily be evacuated to absolute pressure 470Pa by normal pressure, temperature controls at 268 DEG C, and the response time is 45 minutes；Then proceed to evacuation,
Carrying 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, prepare modified poly ester.
The number-average molecular weight of modified poly ester prepared is 29000, by p-phthalic acid segment, ethylene glycol segment and 2-heptan
Base-1,5 pentanediol segment compositions, 2-heptyl-1,5 pentanediol segments are 4.6% with the Mole percent ratio of ethylene glycol segment.
Embodiment 23
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.457 and 2-hexyl-1,5 pentanediols are made into slurry and add in reactor,
Being 55% in concentration, addition is under the catalytic action of the concentrated sulphuric acid of the 0.46% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 239 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification anti-
Should, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.27MPa, and temperature is 255 DEG C, when in esterification
It is esterification terminal when water quantity of distillate reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.41% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 19 minutes,
Addition is the catalytic antimony trioxide of the 0.042% of p-phthalic acid weight and addition is p-phthalic acid weight
Under the effect of the stabilizer NSC 6513 of 0.048%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and temperature controls at 265 DEG C, and the response time is 45 minutes；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, and reaction temperature controls 275
DEG C, in 85 minutes response time, prepare modified poly ester.
The number-average molecular weight of the modified poly ester prepared is 28000, own by p-phthalic acid segment, ethylene glycol segment and 2-
Base-1,5 pentanediol segment compositions, 2-hexyl-1,5 pentanediol segments are 4.41% with the Mole percent ratio of ethylene glycol segment.
Embodiment 24
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.47 and 2-amyl group-1,5 pentanediols are made into slurry and add in reactor,
Concentration is 55wt%, and addition is under the catalytic action of the concentrated sulphuric acid of the 0.48% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.27MPa, and temperature is 245 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification anti-
Should, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.27MPa, and temperature is 259 DEG C, when in esterification
It is esterification terminal when water quantity of distillate reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.67% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 19 minutes,
Addition is the catalytic antimony trioxide of the 0.041% of p-phthalic acid weight and addition is p-phthalic acid weight
Under the effect of the stabilizer triphenyl phosphate of 0.042%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, these rank
Section pressure is steadily evacuated to absolute pressure 485Pa by normal pressure, and temperature controls at 268 DEG C, and the response time is 46 minutes；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,
In 89 minutes response time, prepare modified poly ester.
The number-average molecular weight of the modified poly ester prepared is 29000, by p-phthalic acid segment, ethylene glycol segment and 2-penta
Base-1,5 pentanediol segment compositions, 2-amyl group-1,5 pentanediol segments are 4.67% with the Mole percent ratio of ethylene glycol segment.
Embodiment 25
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
Mixed by p-phthalic acid that mol ratio is 1:1.45 and 2-hexyl-1,5 pentanediol and 2-amyl group-1,4 butanediol
Compound is made into slurry and adds in reactor, wherein 2-hexyl-1, and the mol ratio of 5 pentanediols and 2-amyl group-Isosorbide-5-Nitrae butanediol is 3:1,
Being 55% in concentration, addition is under the catalytic action of the concentrated sulphuric acid of the 0.49% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.26MPa, and temperature is 236 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 258 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.4% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes, is adding
The catalytic antimony trioxide and the addition that enter amount is p-phthalic acid weight 0.042% are p-phthalic acid weight
Under the effect of the stabilizer NSC 6513 of 0.047%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and temperature controls at 265 DEG C, and the response time is 49 minutes；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, and reaction temperature controls 278
DEG C, in 88 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester prepared is 29000, by p-phthalic acid segment, ethylene glycol segment, 2-hexyl-
1,5 pentanediol segment and 2-amyl group-Isosorbide-5-Nitrae butanediol segment composition, 2-hexyl-1,5 pentanediol segments and 2-amyl group-Isosorbide-5-Nitrae fourth two
The summation of alcohol segment is 4.4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 26
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By 2-octyl group-1,6 hexanediol of p-phthalic acid sum that mol ratio is 1:1.45 and 2-amyl group-1,5 pentanediol
Mixture is made into slurry and adds in reactor, wherein 2-octyl group-1,6 hexanediol and 2-amyl group-1, and the mol ratio of 5 pentanediols is 3:
2, it is 60% in concentration, addition is under the catalytic action of the concentrated sulphuric acid of the 0.45% of p-phthalic acid weight, carries out esterification anti-
Should, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 239 DEG C, when in esterification
It is esterification terminal when water quantity of distillate reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification anti-
Should, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.29MPa, and temperature is 255 DEG C, when in esterification
It is esterification terminal when water quantity of distillate reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.6% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes, is adding
The catalytic antimony trioxide and the addition that enter amount is p-phthalic acid weight 0.0423% are p-phthalic acid weight
Under the effect of the stabilizer NSC 6513 of 0.045%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and temperature controls at 265 DEG C, and the response time is 45 minutes；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, and reaction temperature controls 278
DEG C, in 85 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester prepared is 28000, by p-phthalic acid segment, ethylene glycol segment, 2-octyl group-
1,6 hexanediol segment and 2-amyl group-1,5 pentanediol segment compositions, 2-octyl group-1,6 hexanediol segments and 2-amyl group-1,5 penta 2
Alcohol segment is 4.6% with the Mole percent ratio of ethylene glycol segment.
Embodiment 27
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
Mixed by p-phthalic acid that mol ratio is 1:1.45 and 2-hexyl-1,5 pentanediol and 2-amyl group-1,4 butanediol
Compound is made into slurry and adds in reactor, wherein 2-hexyl-1, and the mol ratio of 5 pentanediols and 2-amyl group-Isosorbide-5-Nitrae butanediol is 3:1,
Being 55% in concentration, addition is under the catalytic action of the concentrated sulphuric acid of the 0.49% of p-phthalic acid weight, carries out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.26MPa, and temperature is 236 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.28MPa, and temperature is 258 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.4% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes, is adding
The catalytic antimony trioxide and the addition that enter amount is p-phthalic acid weight 0.042% are p-phthalic acid weight
Under the effect of the stabilizer NSC 6513 of 0.047%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and temperature controls at 265 DEG C, and the response time is 49 minutes；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, and reaction temperature controls 278
DEG C, in 88 minutes response time, prepare modified poly ester.
The number-average molecular weight of modified poly ester prepared is 29000, by p-phthalic acid segment, ethylene glycol segment, 2-hexyl-
1,5 pentanediol segment and 2-amyl group-Isosorbide-5-Nitrae butanediol segment composition, 2-hexyl-1,5 pentanediol segments and 2-amyl group-Isosorbide-5-Nitrae fourth two
The summation of alcohol segment is 4.4% with the Mole percent ratio of ethylene glycol segment.
Embodiment 28
The preparation method of a kind of modified poly ester, specifically includes following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
By p-phthalic acid that mol ratio is 1:1.45 and 2-octyl group-1,3 propylene glycol, 2-amyl group-1,4 butanediol and 2-oneself
Base-1, the mixture of 6 hexanediol is made into slurry and adds in reactor, wherein 2-octyl group-1,3 propylene glycol, 2-amyl group-Isosorbide-5-Nitrae fourth two
Alcohol and 2-hexyl-1, the mol ratio of 6 hexanediol is 3:2:1, is 60% in concentration, and addition is p-phthalic acid weight
Under the catalytic action of the concentrated sulphuric acid of 0.47%, carrying out esterification, esterification is 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 acid and ethylene glycol be made into slurry after add in reactor, carry out esterification,
Esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is 0.27MPa, and temperature is 258 DEG C, when the water in esterification evaporates
It is esterification terminal when output reaches the 92% of theoretical value, obtains ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, add the p-phthalic acid binary alcohol esters of preparation in step (1), right
Phthalic acid binary alcohol esters is 4.71% with the Mole percent ratio of ethylene glycol terephthalate, stirring mixing 18 minutes,
Addition is the catalytic antimony trioxide of the 0.04% of p-phthalic acid weight and addition is p-phthalic acid weight
Under the effect of the stabilizer NSC 6513 of 0.041%, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage, should
Staged pressure is steadily evacuated to absolute pressure 490Pa by normal pressure, and temperature controls at 268 DEG C, and the response time is 49 minutes；Then proceed to
Evacuation, carries out the polycondensation reaction of high vacuum stage of Fig, makes reaction pressure be down to absolute pressure 50Pa, and reaction temperature controls 277
DEG C, in 84 minutes response time, prepare modified poly ester.
The number-average molecular weight of the modified poly ester prepared is 29000, by p-phthalic acid segment, ethylene glycol segment, band side chain
Glycol segment composition, the most branched glycol segment is 2-octyl group-1,3 propylene glycol segments, 2-amyl group-Isosorbide-5-Nitrae butanediol chain
Section and 2-hexyl-1,6 hexanediol segment compositions, branched glycol segment with the Mole percent ratio of ethylene glycol segment is
4.71%.
Embodiment 29
The preparation method of a kind of high uniformity car mould polyester industrial fiber, high uniformity car mould polyester industrial fiber uses porous spray
Filament plate prepares, and on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refers to the hole centre bit of spinneret orifice
On concentration ellipse, concentration ellipse is that series is oval, the major axis conllinear of all ellipses, and short axle conllinear.
As it is shown in figure 1, the ratio of the major axis of ellipse and minor axis length is 1.3, the spacing of adjacent spinneret orifice is equal to spinneret orifice
Guide hole diameter plus 1.5mm, spinneret is circular jetting filament plate, the long axial length that the diameter of circular jetting filament plate is maximum with series ellipse
The difference of degree is 11mm, and a diameter of 2.0mm of guide hole of spinneret orifice, the spray webbing hole count of spinneret is 374, the spinneret orifice of spinneret
Shape of cross section be circular.
The modified poly ester that embodiment 1 prepares is extruded through solid phase polycondensation thickening, metering, porous spinneret, cool down, oils, is drawn
Stretch, thermal finalization and winding, prepare high uniformity car mould polyester industrial fiber, the temperature wherein extruded is 290 DEG C；The pathogenic wind-warm of cooling is
20℃；The oil applying rate oiled is 0.4wt%, and the speed of winding is 2600m/min.
The fracture strength of the high uniformity car mould polyester industrial fiber prepared is 7.9cN/dtex；Line density deviation ratio is
0.6%, fracture strength CV value is 1.8%, and extension at break CV value is 4.5%, and extension at break is 20.0, and at 260 DEG C, melt glues
Degree decline 11%, under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, dry-hot shrinkage is 6.8%.
Embodiment 30
The preparation method of a kind of high uniformity car mould polyester industrial fiber, high uniformity car mould polyester industrial fiber uses porous spray
Filament plate prepares, and on spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, and oval shaped arrangements refers to the hole centre bit of spinneret orifice
On concentration ellipse, concentration ellipse is that series is oval, the major axis conllinear of all ellipses, and short axle conllinear.
As it is shown on figure 3, the ratio of the major axis of ellipse and minor axis length is 1.6, the spacing of adjacent spinneret orifice is equal to spinneret orifice
Guide hole diameter plus 1.5mm, spinneret is circular jetting filament plate, the long axial length that the diameter of circular jetting filament plate is maximum with series ellipse
The difference of degree is 11mm, and a diameter of 2.0mm of guide hole of spinneret orifice, the spray webbing hole count of spinneret is 382, the spinneret orifice of spinneret
Shape of cross section be circular.
The modified poly ester that embodiment 1 prepares is extruded through solid phase polycondensation thickening, metering, porous spinneret, cool down, oils, is drawn
Stretch, thermal finalization and winding, prepare high uniformity car mould polyester industrial fiber, the temperature wherein extruded is 290 DEG C；The pathogenic wind-warm of cooling is
20℃；The oil applying rate oiled is 0.4wt%, and the speed of winding is 2600m/min.
The fracture strength of the high uniformity car mould polyester industrial fiber prepared is 8.2cN/dtex；Line density deviation ratio is
0.7%, fracture strength CV value is 1.7%, and extension at break CV value is 4.8%, and extension at break is 20.0, and at 260 DEG C, melt glues
Degree decline 11%, under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, dry-hot shrinkage is 6.5%.
Comparative example 1
The preparation method of a kind of high uniformity car mould polyester industrial fiber, high uniformity car mould polyester industrial fiber uses porous spray
Filament plate prepares, and on spinneret, the arrangement mode of spinneret orifice is circular arrangement, and it is same that circular arrangement refers to that the hole of spinneret orifice is centrally located at
On heart circle, concentric circular is that series is circular.As in figure 2 it is shown, the spacing of adjacent spinneret orifice adds equal to the guide hole diameter of spinneret orifice
1.5mm, spinneret is circular jetting filament plate, and the difference of the diameter that the diameter of circular jetting filament plate is maximum with series circle is 11mm, spray
The a diameter of 2.0mm of guide hole in silk hole, the spray webbing hole count of spinneret is 370, and the shape of cross section of the spinneret orifice of spinneret is circle
Shape.
The modified poly ester that embodiment 1 prepares is extruded through solid phase polycondensation thickening, metering, porous spinneret, cool down, oils, is drawn
Stretch, thermal finalization and winding, prepare high uniformity car mould polyester industrial fiber, the temperature wherein extruded is 290 DEG C；The pathogenic wind-warm of cooling is
20℃；The oil applying rate oiled is 0.4wt%, and the speed of winding is 2600m/min.
The fracture strength of the high uniformity car mould polyester industrial fiber prepared is 7.9cN/dtex；Line density deviation ratio is 1%,
Fracture strength CV value is 1.9%, and extension at break CV value is 5.3%, and extension at break is 20.1, and at 260 DEG C, melt viscosity declines
11%, under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, dry-hot shrinkage is 6.75%.
When contrasting it can be seen that the effective area of spinneret is identical with embodiment 29, (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 contrasting it can be seen that the effective area of spinneret is identical with embodiment 30, 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,
Embodiment 29 and the prepared fiber linear density deviation ratio of embodiment 30, fracture strength CV value, extension at break CV value are less than comparative example
1, under the conditions of same process is described, the fibre property using the spinneret of spinneret orifice oval shaped arrangements to prepare is better than using spinneret
The spinneret of circular arrangement.
Embodiment 31～33
The preparation method of a kind of high uniformity car mould polyester industrial fiber, uses porous spinneret to prepare, spray webbing on spinneret
The arrangement mode in hole is oval shaped arrangements, and oval shaped arrangements refers to that the hole of spinneret orifice is centrally located on concentration ellipse, concentration ellipse
Oval for series, the major axis conllinear of all ellipses, and short axle conllinear.
Be arranged as long axial symmetry, the major axis of ellipse and the ratio of minor axis length of spinneret orifice are 1.4, between adjacent spinneret orifice
Away from the guide hole diameter equal to spinneret orifice plus 1.6mm, spinneret is circular jetting filament plate, and the diameter of circular jetting filament plate 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.
High uniformity car mould polyester industrial fiber is extruded through metering, porous spinneret, cool down, oils, is stretched, thermal finalization and volume
Around, preparing high uniformity car mould polyester industrial fiber, the temperature wherein extruded is 290 DEG C；The pathogenic wind-warm of cooling is 30 DEG C；Oil is upper
Oil rate is 0.4wt%, and the speed of winding is 3400m/min.
The high uniformity car mould polyester industrial fiber prepared is at 280 DEG C, and melt viscosity declines percent, industrial yarn under room temperature
Mechanical performance data, and under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, industrial yarn xeothermic
Shrinkage factor such as following table.
Embodiment 34～36
The preparation method of a kind of high uniformity car mould polyester industrial fiber, uses porous spinneret to prepare, spray webbing on spinneret
The arrangement mode in hole is oval shaped arrangements, and oval shaped arrangements refers to that the hole of spinneret orifice is centrally located on concentration ellipse, concentration ellipse
Oval for series, the major axis conllinear of all ellipses, and short axle conllinear.
Be arranged as long axial symmetry, the major axis of ellipse and the ratio of minor axis length of spinneret orifice are 1.4, between adjacent spinneret orifice
Away from the guide hole diameter equal to spinneret orifice plus 1.6mm, spinneret is circular jetting filament plate, and the diameter of circular jetting filament plate 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.
High uniformity car mould polyester industrial fiber is extruded through metering, porous spinneret, cool down, oils, is stretched, thermal finalization and volume
Around, preparing high uniformity car mould polyester industrial fiber, the temperature of extrusion is 290 DEG C；The pathogenic wind-warm of cooling is 22 DEG C；The oil applying rate oiled
For 0.7wt%, the speed of winding is 3200m/min.
The high uniformity car mould polyester industrial fiber prepared melt viscosity at 290 DEG C declines percentage ratio, industrial yarn under room temperature
Mechanical performance data, and under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, industrial yarn xeothermic
Shrinkage factor such as following table.
Embodiment 37～39
The preparation method of a kind of high uniformity car mould polyester industrial fiber, uses porous spinneret to prepare, spray webbing on spinneret
The arrangement mode in hole is oval shaped arrangements, and oval shaped arrangements refers to that the hole of spinneret orifice is centrally located on concentration ellipse, concentration ellipse
Oval for series, the major axis conllinear of all ellipses, and short axle conllinear.
Be arranged as long axial symmetry, the major axis of ellipse and the ratio of minor axis length of spinneret orifice are 1.4, between adjacent spinneret orifice
Away from the guide hole diameter equal to spinneret orifice plus 1.6mm, spinneret is circular jetting filament plate, and the diameter of circular jetting filament plate 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.
High uniformity car mould polyester industrial fiber is extruded through metering, porous spinneret, cool down, oils, is stretched, thermal finalization and volume
Around, preparing high uniformity car mould polyester industrial fiber, the temperature wherein extruded is 310 DEG C；The pathogenic wind-warm of cooling is 28 DEG C；Oil is upper
Oil rate is 0.8wt%, and the speed of winding is 3300m/min.
The high uniformity car mould polyester industrial fiber prepared melt viscosity at 270 DEG C declines percent, industrial yarn under room temperature
Mechanical performance data, and under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, industrial yarn xeothermic
Shrinkage factor such as following table.
Embodiment 40～42
The preparation method of a kind of high uniformity car mould polyester industrial fiber, uses porous spinneret to prepare, spray webbing on spinneret
The arrangement mode in hole is oval shaped arrangements, and oval shaped arrangements refers to that the hole of spinneret orifice is centrally located on concentration ellipse, concentration ellipse
Oval for series, the major axis conllinear of all ellipses, and short axle conllinear.
Be arranged as long axial symmetry, the major axis of ellipse and the ratio of minor axis length of spinneret orifice are 1.4, between adjacent spinneret orifice
Away from the guide hole diameter equal to spinneret orifice plus 1.6mm, spinneret is circular jetting filament plate, and the diameter of circular jetting filament plate 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.
High uniformity car mould polyester industrial fiber is extruded through metering, porous spinneret, cool down, oils, is stretched, thermal finalization and volume
Around, preparing high uniformity car mould polyester industrial fiber, the temperature wherein extruded is 300 DEG C；The pathogenic wind-warm of cooling is 28 DEG C；Oil is upper
Oil rate is 0.5wt%, and the speed of winding is 3000m/min.
The high uniformity car mould polyester industrial fiber prepared melt viscosity at 260 DEG C declines percentage ratio, industrial yarn under room temperature
Mechanical performance data, and under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, industrial yarn xeothermic
Shrinkage factor such as following table.
Embodiment 43～45
The preparation method of a kind of high uniformity car mould polyester industrial fiber, uses porous spinneret to prepare, spray webbing on spinneret
The arrangement mode in hole is oval shaped arrangements, and oval shaped arrangements refers to that the hole of spinneret orifice is centrally located on concentration ellipse, concentration ellipse
Oval for series, the major axis conllinear of all ellipses, and short axle conllinear.
Be arranged as long axial symmetry, the major axis of ellipse and the ratio of minor axis length of spinneret orifice are 1.4, between adjacent spinneret orifice
Away from the guide hole diameter equal to spinneret orifice plus 1.6mm, spinneret is circular jetting filament plate, and the diameter of circular jetting filament plate 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.
High uniformity car mould polyester industrial fiber is extruded through metering, porous spinneret, cool down, oils, is stretched, thermal finalization and volume
Around, preparing high uniformity car mould polyester industrial fiber, the temperature wherein extruded is 290 DEG C；The pathogenic wind-warm of cooling is 30 DEG C；Oil is upper
Oil rate is 0.4wt%, and the speed of winding is 3400m/min.
Prepare high uniformity car mould polyester industrial fiber at 280 DEG C, melt viscosity, the mechanical property of industrial yarn under room temperature
Data, and under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, the dry-hot shrinkage of industrial yarn is as follows
Table.
Embodiment 46～48
The preparation method of a kind of high uniformity car mould polyester industrial fiber, uses porous spinneret to prepare, spray webbing on spinneret
The arrangement mode in hole is oval shaped arrangements, and oval shaped arrangements refers to that the hole of spinneret orifice is centrally located on concentration ellipse, concentration ellipse
Oval for series, the major axis conllinear of all ellipses, and short axle conllinear.
Be arranged as long axial symmetry, the major axis of ellipse and the ratio of minor axis length of spinneret orifice are 1.4, between adjacent spinneret orifice
Away from the guide hole diameter equal to spinneret orifice plus 1.6mm, spinneret is circular jetting filament plate, and the diameter of circular jetting filament plate 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.
High uniformity car mould polyester industrial fiber is extruded through metering, porous spinneret, cool down, oils, is stretched, thermal finalization and volume
Around, preparing high uniformity car mould polyester industrial fiber, the temperature wherein extruded is 310 DEG C；The pathogenic wind-warm of cooling is 30 DEG C；Oil is upper
Oil rate is 0.7wt%, and the speed of winding is 3200m/min.
The high uniformity car mould polyester industrial fiber prepared melt viscosity at 280 DEG C declines percent, industrial yarn under room temperature
Mechanical performance data, and under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, industrial yarn xeothermic
Shrinkage factor such as following table.
Embodiment 49～51
The preparation method of a kind of high uniformity car mould polyester industrial fiber, uses porous spinneret to prepare, spray webbing on spinneret
The arrangement mode in hole is oval shaped arrangements, and oval shaped arrangements refers to that the hole of spinneret orifice is centrally located on concentration ellipse, concentration ellipse
Oval for series, the major axis conllinear of all ellipses, and short axle conllinear.
Be arranged as long axial symmetry, the major axis of ellipse and the ratio of minor axis length of spinneret orifice are 1.4, between adjacent spinneret orifice
Away from the guide hole diameter equal to spinneret orifice plus 1.6mm, spinneret is circular jetting filament plate, and the diameter of circular jetting filament plate 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.
High uniformity car mould polyester industrial fiber is extruded through metering, porous spinneret, cool down, oils, is stretched, thermal finalization and volume
Around, preparing high uniformity car mould polyester industrial fiber, the temperature wherein extruded is 300 DEG C；The pathogenic wind-warm of cooling is 25 DEG C；Oil is upper
Oil rate is 0.6wt%, and the speed of winding is 2800m/min.
The high uniformity car mould polyester industrial fiber melt viscosity at 280 DEG C prepared, the mechanical property of industrial yarn under room temperature
Data, and under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, the dry-hot shrinkage of industrial yarn is as follows
Table.
Embodiment 52～57
The preparation method of a kind of high uniformity car mould polyester industrial fiber, uses porous spinneret to prepare, spray webbing on spinneret
The arrangement mode in hole is oval shaped arrangements, and oval shaped arrangements refers to that the hole of spinneret orifice is centrally located on concentration ellipse, concentration ellipse
Oval for series, the major axis conllinear of all ellipses, and short axle conllinear.
Be arranged as long axial symmetry, the major axis of ellipse and the ratio of minor axis length of spinneret orifice are 1.4, between adjacent spinneret orifice
Away from the guide hole diameter equal to spinneret orifice plus 1.6mm, spinneret is circular jetting filament plate, and the diameter of circular jetting filament plate 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.
High uniformity car mould polyester industrial fiber is extruded through metering, porous spinneret, cool down, oils, is stretched, thermal finalization and volume
Around, preparing high uniformity car mould polyester industrial fiber, the temperature wherein extruded is 320 DEG C；The pathogenic wind-warm of cooling is 30 DEG C；Oil is upper
Oil rate is 0.8wt%, and the speed of winding is 3400m/min.
The high uniformity car mould polyester industrial fiber prepared melt viscosity at 280 DEG C declines percentage ratio, industrial yarn under room temperature
Mechanical performance data, and under the test condition that temperature is 177 DEG C × 10min × 0.05cN/dtex, industrial yarn xeothermic
Shrinkage factor such as following table.
Claims (10)
1. a high uniformity car mould polyester industrial fiber, is characterized in that: described high uniformity car mould polyester industrial fiber is gathered by modification
Ester spinning after solid-phase tack producing obtains；The material of described high uniformity car mould polyester industrial fiber is modified poly ester, described modified poly ester
Being made up of p-phthalic acid segment, ethylene glycol segment and the dihydroxylic alcohols segment containing side chain, the described dihydroxylic alcohols segment containing side chain is
Refer on a non-end group carbon being positioned in dihydroxylic alcohols segment of side chain and side chain is the linear carbon chain containing 5-10 carbon atom two
Unit's alcohol segment；Described high uniformity car mould polyester industrial fiber is at 260～290 DEG C, and melt viscosity declines 10-20%, in temperature
Being under the test condition of 177 DEG C × 10min × 0.05cN/dtex, dry-hot shrinkage is 7.0 ± 0.5%；Described high uniformity car
The fracture strength of mould polyester industrial fiber >=7.7cN/dtex line density deviation ratio≤1.0%, fracture strength CV value≤2.0%, disconnected
Split elongation CV value≤5.5%.
A kind of high uniformity car mould polyester industrial fiber the most according to claim 1, it is characterised in that described high uniformity car
The extension at break 19.0 ± 1.5% of mould polyester industrial fiber；The number-average molecular weight of described modified poly ester is 15000-30000.
A kind of high uniformity car mould polyester industrial fiber the most according to claim 1, it is characterised in that described containing side chain two
Unit's alcohol segment is that 2-amyl group-1,3 propylene glycol segment, 2-hexyl-1,3 propylene glycol segment, 2-heptyl-1,3 propylene glycol segment, 2-are pungent
Base-1,3 propylene glycol segment, 2-nonyl-1,3 propylene glycol segment, 2-decyl-1,3 propylene glycol segment, 2-amyl group-1,4 butanediol chain
Section, 2-hexyl-1,4 butanediol segment, 2-heptyl-1,4 butanediol segment, 2-octyl group-1,4 butanediol segment, 2-nonyl-1,4
Butanediol segment, 2-decyl-1,4 butanediol segment, 2-amyl group-1,5 pentanediol segment, 2-hexyl-1,5 pentanediol segment, 2-
Heptyl-1,5 pentanediol segment, 2-octyl group-1,5 pentanediol segment, 2-nonyl-1,5 pentanediol segment, 2-decyl-1,5 pentanediol
Segment, 2-amyl group-1,6 hexanediol segment, 2-hexyl-1,6 hexanediol segment, 2-heptyl-1,6 hexanediol segment, 2-octyl group-1,
More than one in 6 hexanediol segments, 2-nonyl-1,6 hexanediol segment or 2-decyl-1,6 hexanediol segment；Described containing side chain
The Mole percent ratio of dihydroxylic alcohols segment and ethylene glycol segment be 2～5%.
4. the preparation method of a kind of high uniformity car mould polyester industrial fiber as according to any one of claim 1-3, its feature
It is: modified poly ester is extruded through solid phase polycondensation thickening, metering, porous spinneret, cool down, oils, stretched, thermal finalization and winding,
Prepare high uniformity car mould polyester industrial fiber；
On described porous spinneret, the arrangement mode of spinneret orifice is oval shaped arrangements, and described oval shaped arrangements refers to the hole of spinneret orifice
Being centrally located on concentration ellipse, described concentration ellipse is that series is oval, the major axis conllinear of all ellipses, and short axle conllinear；
The preparation process of modified poly ester comprises the following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
After p-phthalic acid is made into slurry with the dihydroxylic alcohols containing side chain, under the catalytic action of concentrated sulphuric acid, carry out esterification,
Obtain p-phthalic acid binary alcohol esters；The described dihydroxylic alcohols containing side chain is the non-end group carbon that side chain is positioned in dihydroxylic alcohols segment
Upper and that side chain is the linear carbon chain containing 5-10 carbon atom dihydroxylic alcohols；
(2) preparation of ethylene glycol terephthalate:
After p-phthalic acid and ethylene glycol are made into slurry, carry out esterification, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, adding the p-phthalic acid binary alcohol esters of preparation in step (1), stirring is mixed
Close, under the effect 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, prepares modified poly ester.
The preparation method of high uniformity car mould polyester industrial fiber the most according to claim 4, it is characterised in that described modification
Prepared by polyester concretely comprises the following steps:
(1) preparation of p-phthalic acid binary alcohol esters:
P-phthalic acid and the dihydroxylic alcohols containing side chain are made into slurry add in reactor, under the catalytic action of concentrated sulphuric acid, enter
Row esterification, esterification is compressive reaction in nitrogen atmosphere, and moulding pressure is normal pressure～0.3MPa, and temperature is 180～240
DEG C, it is esterification terminal when the water quantity of distillate in esterification reaches more than the 90% of theoretical value；Obtain p-phthalic acid
Binary alcohol esters；
(2) preparation of ethylene glycol terephthalate:
Adding in reactor after p-phthalic acid and ethylene glycol are made into slurry, carry out esterification, esterification is in blanket of nitrogen
Enclosing middle compressive reaction, moulding pressure is normal pressure～0.3MPa, and temperature is 250～260 DEG C, when the water quantity of distillate in esterification reaches
To theoretical value more than 90% time be esterification terminal, obtain ethylene glycol terephthalate；
(3) preparation of modified poly ester:
After esterification in step (2) terminates, adding the p-phthalic acid binary alcohol esters of preparation in step (1), stirring is mixed
Close 15-20 minute, under the effect of catalyst and stabilizer, under conditions of negative pressure, start the polycondensation reaction in coarse vacuum stage,
This staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature controls 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, response time 50～90 minutes, prepares modified poly ester；
Again through pelletizing, modified poly ester being obtained Modified polyester chips, obtained polyester slice is viscosified by solid phase polycondensation, makes polyester
The intrinsic viscosity of section brings up to 1.0～1.2dL/g, is high viscous section；Again through metering, porous spinneret extrusion, cooling, on
Oil, stretching, thermal finalization and winding, prepare high uniformity car mould polyester industrial fiber；
Spinning main technologic parameters is:
The temperature of described extrusion is 290～320 DEG C；
The pathogenic wind-warm of described cooling is 20～30 DEG C；
The described oil applying rate oiled is 0.4～0.8wt%；
The speed of described winding is 2600～3400m/min.
The preparation method of a kind of high uniformity car mould polyester industrial fiber the most according to claim 5, it is characterised in that described
In step (1), p-phthalic acid is 1:1.3-1.5 with the mol ratio of the dihydroxylic alcohols containing side chain；Concentrated sulphuric acid addition is to benzene two
The 0.3-0.5% of formic acid weight；The concentration of described concentrated sulphuric acid is 50-60wt%；In described step (2), p-phthalic acid and second
The mol ratio of glycol is 1:1.2～2.0；In described step (3), described p-phthalic acid binary alcohol esters and p-phthalic acid second two
The Mole percent ratio of alcohol ester is 2～5%；Described catalyst is antimony oxide, antimony glycol or antimony acetate, and catalyst adds
Amount is the 0.01%～0.05% of p-phthalic acid gross weight；Described stabilizer is triphenyl phosphate, trimethyl phosphate or phosphorous
Acid trimethyl, stabilizer addition is the 0.01%～0.05% of described p-phthalic acid gross weight.
The preparation method of a kind of high uniformity car mould polyester industrial fiber the most according to claim 5, it is characterised in that described
Dihydroxylic alcohols containing side chain is 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, 2-decyl-1,3 propylene glycol, 2-amyl group-1,4 butanediol, 2-hexyl-1,4 butanediol, 2-
Heptyl-1,4 butanediol, 2-octyl group-1,4 butanediol, 2-nonyl-1,4 butanediol, 2-decyl-1,4 butanediol, 2-amyl group-1,5
Pentanediol, 2-hexyl-1,5 pentanediol, 2-heptyl-1,5 pentanediol, 2-octyl group-1,5 pentanediol, 2-nonyl-1,5 pentanediol, 2-
Decyl-1,5 pentanediols, 2-amyl group-1,6 hexanediol, 2-hexyl-1,6 hexanediol, 2-heptyl-1,6 hexanediol, 2-octyl group-1,6
More than one in hexanediol, 2-nonyl-1,6 hexanediol or 2-decyl-1,6 hexanediol.
The preparation method of a kind of high uniformity car mould polyester industrial fiber the most according to claim 4, it is characterised in that described
Porous spinneret is circular jetting filament plate or elliptical spinneret plate；The major axis that the diameter of described circular jetting filament plate is maximum with series ellipse
The difference of length is more than 10mm, and the difference of the long axis length that described elliptical spinneret plate is maximum with series ellipse is more than 10mm.
The preparation method of a kind of high uniformity car mould polyester industrial fiber the most according to claim 4, it is characterised in that described
On porous spinneret spinneret orifice be arranged as major axis and/or short axial symmetry, the spacing of adjacent spinneret orifice is more than or equal to spinneret orifice
Guide hole diameter adds 1.5mm；Oval major axis is 1.3～1.8 with the ratio of minor axis length.
The preparation method of a kind of high uniformity car mould polyester industrial fiber the most according to claim 4, it is characterised in that institute
State the guide hole a diameter of 1.5～2.5mm of spinneret orifice；The spray webbing hole count of described spinneret is more than or equal to 192, the spray of described spinneret
The shape of cross section of silk micropore is circle, square, rhombus, yi word pattern, triangular form, trilobal cross, hollow type or platypelloid type.
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