CN105648570A - Low-color-difference polyester wool-like different-shrinkage complex yarn and preparation method thereof - Google Patents
Low-color-difference polyester wool-like different-shrinkage complex yarn and preparation method thereof Download PDFInfo
- Publication number
- CN105648570A CN105648570A CN201511018915.6A CN201511018915A CN105648570A CN 105648570 A CN105648570 A CN 105648570A CN 201511018915 A CN201511018915 A CN 201511018915A CN 105648570 A CN105648570 A CN 105648570A
- Authority
- CN
- China
- Prior art keywords
- polyester
- low
- low aberration
- wool
- composite filament
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/83—Alkali metals, alkaline earth metals, beryllium, magnesium, copper, silver, gold, zinc, cadmium, mercury, manganese, or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
- C08G63/86—Germanium, antimony, or compounds thereof
- C08G63/866—Antimony or compounds thereof
-
- 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
- C08G63/88—Post-polymerisation treatment
- C08G63/90—Purification; Drying
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D7/00—Collecting the newly-spun products
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
Abstract
The invention relates to low-color-difference polyester wool-like different-shrinkage complex yarn and a preparation method thereof. The low-color-difference polyester wool-like different-shrinkage complex yarn is prepared through carrying out fiber intermingling on low-color-difference polyester POY (Pre-Oriented Yarn) and low-color-difference polyester FDY (Fully Drawn Yarn), wherein the low-color-difference polyester POY forms small yarn loops which surround the low-color-difference polyester FDY; the low-color-difference polyester POY and the low-color-difference polyester FDY are made from polyester through carrying out dissolving and washing and then carrying out spinning. The low-color-difference polyester wool-like different-shrinkage complex yarn has the rupture strength not lower than 3.0cN/dtex, the breaking elongation of 40.0+/-3.0%, the crimp contraction of 5.50+/-3.0%, the interlacing degree of 95+/-5/m, the fiber number of 150dtex to 300dtex and the color difference [delta]E smaller than 0.200. According to the low-color-difference polyester wool-like different-shrinkage complex yarn and the preparation method thereof, ethylene glycol magnesium is relatively mild and has a very small thermal degradation coefficient, and the oligomers are reduced during polymerization and are further reduced during washing, so that during the dyeing and postprocessing thermosetting of polyester fibers, the amount of the oligomers migrating to the outside of the fibers from the inside is reduced, the occurrence of color spots and streaks is reduced, and the level dyeability and rubbing fastness of the fibers are guaranteed.
Description
Technical field
The invention belongs to polyester preparing technical field, relate to a kind of low aberration polyester Wool-Like abnormal contraction composite filament and preparation method thereof,Particularly a kind of polycondensation catalyst adopt the mixture of ethylene glycol magnesium and antimony glycol and polyester slice through water with dissolve and wash away agent and exist120～130 DEG C, low aberration polyester Wool-Like abnormal contraction composite filament of brew, washing and preparation method thereof under 0.2～0.3MPa condition.
Background technology
PETG (PET) is a kind of polymer of function admirable, PET is high with its modulus, intensity is high, well-pressed,Good, the pure health of conformality, barrier property are good etc., are widely used in the fields such as fiber, bottle packaging, film and sheet material, produceAmount cumulative year after year, position in industry significantly promotes.
PET belongs to the large molecule of symmetric straight chain, and strand does not contain side-chain radical, and regularity is very good, the glass of this structureGlass transition temperature is higher, need at very high temperature, dye, and promotes the diffusion of dye molecule to fibrous inside. In addition, PETStrand regular, good crystallinity, strand is arranged closely, and the polarity of not having an effect with dye molecule on strandGroup, makes the colouring of polyester fiber more difficult. Owing to there is no hydrophilic radical in its molecule, hygroscopicity is very poor, and this causes teryleneDyeing more difficult. The main high-temperature and high pressure dyeing process method of terylene disperse dyeing
Oligomer in polyester fiber is a kind of low-molecular-weight ester or ether, mainly refers to that the degree of polymerization is less than 10 oligomer, two sweetAlcohol is to produce with the form of accessory substance. Wherein oligomer is divided into linear oligomerization thing and cyclic oligomer, wherein with ring-type aggressiveness spyBe not that cyclic trimer is in the majority, oligomer is mainly concerned with heterogeneous nucleation, spinning processing, dyeing etc., the performance to polyester and afterRoad processing causes certain harmful effect. Ethylene glycol terephthalate polymer (PET) approximately, containing oligomer 3-4%, is worked as fiberSurface occurs that oligomer will make troubles to dyeing and rear processing. Control when the diffusing out of oligomer the most easily occurs in dyeingThe gentle holding stage of temperature rise. In the time of cooling, the same as with dyestuff the solubility with temperature reduction of oligomer in water sharply reduces,Therefore can crystallization, the dyestuff of separating out and oligomer are attached to the fiber surface utmost point and are not easy to wash away, thereby give dyeing and rear processingBring a lot of troubles, in dyeing course, dyestuff and the oligomer of gathering stick to fiber surface, occur dyestuff color dot, spot,The phenomenons such as look flower. Be deposited in the pipeline and valve of overflow dyeing machine, hinder the circulation of liquid stream, cause dyeing difficulty. Elimination oligomer closesKey is to eliminate oligomer cyclic trimer and diethylene glycol (DEG), is the generation that reduces oligomer in polymerization process on the one hand, the opposing partyFace is to remove before dyeing or in dyeing.
Wool-Like abnormal contraction composite filament is the long filament with different potential shrinkages, i.e. high-shrinkage filament POY and low contractile filaments FDYThrough the composite filament of mixed fine processing composition, the main feature of the different contraction mixed fiber composite of PET silk: high loft and soft feel. PETWool-Like abnormal contraction composite filament outer existing similar with common long filament. Due to the difference of two component shrinkage factors, after heat treatment, high receiptsContracting part forms the core silk of clear-cut, become the skeleton of silk, and low constriction forms tiny wire ring around core silk, itsBe exactly like textured filament in appearance. Gloss is soft. Due to bulk and surperficial many wire rings of PET Wool-Like abnormal contraction composite filament,Eliminate the aurora defect of chemical fiber wire fabric. Excellent warmth retention property. The high loft of the different contraction mixed fiber composite of PET silk, increases fineSpace between dimension. Cause the air content in the different contraction mixed fiber composite of PET silk fabrics to increase.
Summary of the invention
The object of this invention is to provide a kind of low aberration polyester Wool-Like abnormal contraction composite filament and preparation method thereof, is that a kind of polycondensation is urgedAgent adopts polyester and low aberration polyester Wool-Like abnormal contraction composite filament and the preparation thereof of the mixture of ethylene glycol magnesium and antimony glycolMethod. It is polycondensation catalyst that the present invention adopts the mixture of ethylene glycol magnesium and antimony glycol, and thermal degradation is reduced to minimum, andPolyester slice is through water and dissolve and wash away agent at 130 DEG C, brew, washing under 0.3MPa condition; Reduce oligomer, diethylene glycol (DEG) content to poly-Ester composite filament dyeing impact.
The low aberration polyester of one of the present invention Wool-Like abnormal contraction composite filament, for described polyester is that terephthalic acid (TPA) and ethylene glycol are through esterChange and under the mixture through catalytic effect of ethylene glycol magnesium and antimony glycol polycondensation, granulation and dissolve and wash away after spinning processing make; Described lowAberration Wool-Like abnormal contraction composite filament is that low aberration polyester POY silk and low aberration polyester FDY silk are processed the compound of composition through mixed fibreSilk, described low aberration polyester POY silk forms tiny wire ring and is centered around around described low aberration polyester FDY silk; Described low aberrationPolyester POY silk and low aberration polyester FDY silk are that described low aberration polyester Wool-Like is different via polyester spinning and obtaining after dissolveing and washing awayFracture strength >=the 2.1cN/dtex of contraction composite filament, elongation at break is 15.0 ± 2.0%, crimp contraction is 5.50 ± 3.0%, netNetwork degree is 90 ± 5/m, fiber number: 150-300dtex, and aberration Δ E is less than 0.200;
Described industry is with in the section of polyester, and oligomer mass percentage content is less than 0.5%, the mass percentage content of diethylene glycol (DEG)Be less than 0.5%;
The molecular formula of described ethylene glycol magnesium is Mg (OCH2CH2OH)2；
Described dissolve and wash away the section that refers to after granulation through water with dissolve and wash away agent 120～130 DEG C with 0.2～0.3MPa condition under brew and washingWash.
In polyester fiber dyeing and rear processing, affect the factor that surface oligomers separates out a lot, mainly contain temperature and time etc. because ofElement. Improve dyeing temperature by the migration of aggravation oligomer, particularly, in the time having some auxiliary agent or dyestuff to exist, migration velocity improvesFaster. The time of dye liquor circulation continuous is longer, and oligomer increases to the amount of external migration in fiber, often cold cycling andThe existence of a little auxiliary agents, dyestuff can greatly aggravate oligomer shift out and deposit. The temperature and time of heat setting is simultaneously to oligomerMigration velocity and migration amount have a significant impact. Concerning synthetic fibers dyeing and finishing processing, heat setting is an extremely important operation, itsMain purpose be eliminate existing fine wrinkle on fabric and improve the dimensional stability of fabric and improve fabric brute force, feel, riseThe performances such as hair balling-up and surfacing. But, in yarn dyed fabric shaping process, often there is such phenomenon, after heat settingEasily there is color spot and barriness in fabric face, level-dyeing property and crock fastness also significantly decline, especially for Polyester Fabric of Ultra-fine Fibre under Alkali Condition,Affect particularly seriously, oligomer migration from inside to outside under heat effect is one of the main reasons. Existing technology all concentrates on and dyesColour circle joint solves the impact of oligomer on dyeing, and this is that one is controlled calibration method, only solves from source to be only to effect a permanent cureAt all.
Adopt ethylene glycol magnesium and antimony glycol mixture as polycondensation catalyst, ethylene glycol magnesium belongs to a comparatively gentle class, its heatDegradation coefficient is very little, and the side reaction causing in course of reaction is less, has reduced the generation of oligomer in process. CauseThe principal element of thermal degradation is high temperature and catalyst, and high temperature is that response intensity is too high, causes degraded to be accelerated, and has produced end carboxyl,Also make cyclic oligomer increase simultaneously; Catalyst is relevant to the degradation reaction constant of catalyst, in polycondensation process, and catalystEffect be not only can catalysis to generate main reaction, thereby speed and the output of impact reaction, simultaneously can also catalytic thermal degraded and etherKey generates, and increases the content of cyclic oligomer and diethylene glycol (DEG).
The line density deviation ratio of a kind of low aberration polyester Wool-Like abnormal contraction composite filament as above is ± 2.5%, fracture strength CVValue≤5.0%, extension at break CV value≤10.0%, boiling water shrinkage is 10.0 ± 1.0%, crimp contraction coefficient of variation CV value≤ 10.0%, oil content is 1.0 ± 0.2%, fiber number: 75-150dtex; Line density deviation ratio≤0.2% of low aberration polyester POY silk,Fracture strength >=2.6cN/dtex, fracture strength CV value≤3.0%, elongation at break is 90.0 ± 10.0%, extension at break CV value≤ 6.0%. ; Line density deviation ratio≤0.5% of low aberration polyester FDY silk, fracture strength >=3.8cN/dtex, fracture strength CV value≤ 5.0%, elongation at break is 33.0 ± 3.0%, extension at break CV value≤10.0%, and yarn unevenness CV≤2.00%, boiling water is receivedShrinkage 7.5 ± 0.5%, oil content 0.90 ± 0.20%.
The low aberration polyester of one as above Wool-Like abnormal contraction composite filament, in the mixture of described ethylene glycol magnesium and antimony glycol,Ethylene glycol magnesium and antimony glycol mass ratio are 2～3:1.
The present invention also provides a kind of preparation method of low aberration polyester Wool-Like abnormal contraction composite filament, a kind of low aberration polyester simulate woolThe preparation method of type abnormal contraction composite filament, for terephthalic acid (TPA) and ethylene glycol are through esterification with in the mixing of ethylene glycol magnesium and antimony glycolUnder thing catalytic action, polycondensation makes polyester, then obtains polyester slice through pelletizing, after then polyester slice being dissolved and washed away, makes polyester;By polyester through measuring, extrude, cooling, oil and reel, make low aberration modified poly ester POY silk; By polyester slice through metering,Extrude, cooling, oil, stretching, thermal finalization and coiling, make low aberration polyester FDY silk; Then by low aberration polyester POYSilk and low aberration polyester FDY silk through plying network, add hot-stretch, false twisting, thermal finalization and coiling and molding make low aberration polyester imitateWool type abnormal contraction composite filament; Main technique is:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Perfectly straightStream electricity, starting voltage 6～10VV, cathode-current density is 150～200mA, electrolysis 10～12 hours 50～60 DEG C time, electrolysisAfter finishing, take out electrode, obtain white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol after being driedMagnesium;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt terephthalic acid (TPA) and ethylene glycol as raw material, add anti-ether agent, carry out esterification after being made into uniform sizing material, obtainEsterification products; Esterification is pressurizeed in nitrogen atmosphere, and pressure is controlled at normal pressure～0.3MPa, and temperature is at 250～260 DEG C, esterificationWhat water quantity of distillate reached theoretical value more than 90% is esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction low vacuum stage, add catalyst and stabilizing agent in esterification products, starts contracting under the condition of negative pressurePoly-reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature is controlled at 260～270 DEG C, when reactionBetween be 30～50 minutes; Described catalyst is the mixture of ethylene glycol magnesium and antimony glycol;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and reaction pressure is fallenBe less than 100Pa to absolute pressure, reaction temperature is controlled at 275～280 DEG C, 50～90 minutes reaction time;
Make polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Described polyester slice through water with dissolve and wash away agent 120～130 DEG C with 0.2～0.3MPa condition under brew 3-5 hour, by washing;Obtain polyester.
(4) spinning processing main technologic parameters:
A. polyester POY yarn spinning technique;
Spinning temperature: 280-290 DEG C;
Chilling temperature: 18-22 DEG C;
Winding speed: 3200-3600m/min;
B. polyester FDY yarn spinning technique:
Spinning temperature: 280-290 DEG C;
Chilling temperature: 20-25 DEG C;
Network pressure: 0.20-0.30Mpa;
One roller speed: 2200-2600m/min;
One roll temperature: 75-85 DEG C;
Two roller speed: 3600-3900m/min;
Two roll temperatures: 115-135 DEG C;
Winding speed: 3600-3800m/min;
C. composite filament processing technology:
Spin fast 400-800m/min;
Sizing over feed rate(OFR) 3.5-5.50%;
Coiling over feed rate(OFR) 2.5-5.0;
T1：180-220℃；
T2：150-180℃；
DR：1.6-1.8；
D/Y:1.6-2.0；
Network pressure: 0.05-0.3mpa;
High heat setting temperature in the high elongation at tear of POY, higher chilling temperature and DTY process is simulate woolThe high elongation at tear of type abnormal contraction composite filament provides technical support.
The preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament as above, described ethylene glycol and described to benzene twoThe mol ratio of formic acid is 1.2～2.0:1.
The preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament as above, described ethylene glycol magnesium and antimony glycolMixture in, ethylene glycol magnesium and antimony glycol mass ratio are 2～3:1; Described catalyst amount is described terephthalic acid (TPA) quality0.01％～0.05％。
The preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament as above, described stabilizing agent is selected from phosphoric acid triphenOne in ester, trimethyl phosphate and Trimethyl phosphite, stabilizing agent dosage is described terephthalic acid (TPA) weight0.01%～0.05%. Stabilizing agent is mainly taking phosphate as main, and Main Function is the free radical that catching reaction produces in polymerization process,Reduce side reaction.
The preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament as above, described water and the mass ratio that dissolves and washes away agentExample is 100:3～4, polyester slice and water and the ratio that dissolves and washes away agent, and solid-to-liquid ratio is 1:5-10; It is described that to dissolve and wash away agent be ethylene glycol one secondOne in ether, propyl cellosolve and ethylene glycol monobutyl ether (EGMBE) adds a small amount of agent that dissolves and washes away in water, dissolves and washes away agent water-soluble, withTime also the most of low molecular ether of solubilized and ester, be conducive to improve the effect of washing and the minimizing of oligomer.
The preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament as above, described washing refers to polyester after brew70～80 DEG C of hot water wash 10～15min for section, then clean with cold water, and Drying and cooling is for subsequent use.
The preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament as above, described anti-ether agent is sodium acetate and vinegarOne in acid calcium, anti-ether agent consumption is 0.01%～0.05% of described terephthalic acid (TPA) weight. Anti-ether agent is a small amount of by addingNaAc reduces the generation of ether under acid condition, thereby has reduced the activity of glycol reaction generation diethylene glycol (DEG).
The object of this invention is to provide a kind of low aberration polyester Wool-Like abnormal contraction composite filament, adopt a relatively mild class polycondensation catalysisAgent ethylene glycol magnesium, the less thermal degradation in the less and process of the less side reaction that causes in course of reaction, has reducedThe generation of oligomer in process. Polyester slice is through water and dissolve and wash away agent at 130 DEG C, and under 0.3MPa condition, brew is conducive to improveThe effect of washing and the minimizing of oligomer. The minimizing of oligomer, makes in polyester fiber dyeing and rear processing heat setting oligomerIn fiber, reduce to the amount of external migration, reduced color spot and barriness and occurred, ensured fiber level-dyeing property and crock fastness.
Beneficial effect:
● adopt ethylene glycol magnesium and antimony glycol mixture as polycondensation catalyst, ethylene glycol magnesium belongs to a comparatively gentle class, itsThermal degradation coefficient is very little, and the side reaction causing in course of reaction is less, reduced at process middle-end carboxyl andThe generation of oligomer.
● the oligomer mass percentage content of polyester slice is less than 0.5%, and the mass percentage content of diethylene glycol (DEG) is less than 0.5%,Be conducive to further improve the quality of fiber.
● polyester slice through water with dissolve and wash away agent 120～130 DEG C with 0.2～0.3MPa condition under brew be conducive to improve wash effectThe minimizing of fruit and oligomer.
● anti-ether agent is by adding a small amount of NaAc to reduce the generation of ether under acid condition, thereby reduced glycol reaction generationThe activity of diethylene glycol (DEG).
● the minimizing of oligomer in polymerization process, dissolve and wash away oligomer in process and further reduce, make polyester fiber dyeing and after addIn work heat setting, oligomer reduces to the amount of external migration in fiber, has reduced color spot and barriness and has occurred, has ensuredFiber level-dyeing property and crock fastness.
● bulk and surperficial many wire rings of the Wool-Like abnormal contraction composite filament of gained of the present invention, eliminate chemical fiber wire fabricAurora defect, has excellent warmth retention property, and the high loft of Wool-Like abnormal contraction composite filament, has increased between fiberSpace.
Detailed description of the invention
Below in conjunction with detailed description of the invention, further set forth the present invention. Should be understood that these embodiment are only for illustrating the present inventionBe not used in and limit the scope of the invention. In addition should be understood that after having read the content of the present invention's instruction those skilled in the artCan make various changes or modifications the present invention, these equivalent form of values fall within the model that the application's appended claims limits equallyEnclose.
A preparation method for low aberration polyester Wool-Like abnormal contraction composite filament, by polyester through measuring, extrude, cooling, oil andReel, make low aberration modified poly ester POY silk; By polyester slice through measuring, extrude, cooling, oil, stretching, thermal finalizationAnd coiling, make low aberration polyester FDY silk; Then by low aberration polyester POY silk and low aberration polyester FDY silk through plying netNetwork, add hot-stretch, false twisting, thermal finalization and coiling and molding and make low aberration polyester Wool-Like abnormal contraction composite filament.
1, dyestuff:
Disperse brilliant blue 2BLN, 5% (o.w.f)
2, dyeing:
Fiber enters to dye insulation 10～15min at 70～80 DEG C, 1.0～2.0 DEG C/min of heating rate, 120～130 DEG C of insulations 40～60Min, cooling, 70～80 DEG C of reduction cleaning 20～30min.
3, the mensuration of dye uptake
Dye by above-mentioned technique, and draw and dye front liquid respectively, the each 2ml of Liquid Residue, in 10ml volumetric flask, adds acetone4ml, fully dissolves dyestuff. To scale, then use spectrophotometric instrumentation λ with distilled water dilutingmax, dyestuff before and after time dyeingAbsorbance A 0, A1 be:
Dye uptake (%)=(l mono-A1/A0) × 100%
In formula: A0---dyes the absorbance of front liquid
The absorbance of A1---Liquid Residue
4, the mensuration of dyefastness
Press GB3920-83, GB251-64, GB3921-83 test
5, the mensuration of tinctorial yield and aberration
Adopt the test of color measurement and color match instrument.
6, the mensuration of the apparent colour degree of depth (K/S)
Utilize storehouse Bel's card-Munch (kubelka-munk) function to calculate: in K/S=(1-R) 2//2R. formula, K is testedThe absorption coefficient of object; S is the scattering coefficient of testee; Reflectivity when R is testee infinite thickness. ApplicationThe test of SF600XDatacolor color measurement and color match instrument, every sample, zones of different test 5 times, is got its mathematical mean.
Embodiment 1
A preparation method for low aberration polyester Wool-Like abnormal contraction composite filament, main technique comprises:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite;Logical direct current, starting voltage 6V, cathode-current density is 150mA, electrolysis 10 hours 50 DEG C time, gets after electrolysis finishesGo out electrode, obtain white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol magnesium after being dried;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Esterification:
Adopt terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 1.2:1, adds anti-Ether agent sodium acetate, sodium acetate consumption is 0.01% of terephthalic acid (TPA) weight, carries out esterification after being made into uniform sizing material,To esterification products; Esterification is pressurizeed in nitrogen atmosphere, and pressure is controlled at normal pressure, and temperature is at 250 DEG C, and esterification water distillatesIt is esterification terminal that amount reaches 91% of theoretical value;
Polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the polycondensation reaction low vacuum stage, add catalyst and stabilizing agent triphenyl phosphate in esterification products, and catalyst amount is0.01% of terephthalic acid (TPA) quality, triphenyl phosphate consumption is 0.01% of terephthalic acid (TPA) weight, under the condition of negative pressureStart polycondensation reaction, this staged pressure is steadily evacuated to absolute pressure 498Pa by normal pressure, and temperature is controlled at 260 DEG C, when reactionBetween be 30 minutes; Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, and ethylene glycol magnesium and antimony glycol mass ratio are 2:1;
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, and reaction pressure is down to definitelyPressure 96Pa, reaction temperature is controlled at 275 DEG C, 50 minutes reaction time; Make polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent ethylene glycol monoethyl ether 120 DEG C with 0.2MPa condition under brew 3 hours, by washingWash, i.e. 70 DEG C of hot water wash 10min for polyester slice after brew, then clean with cold water, and Drying and cooling is for subsequent use; GatheredEster, water is 100:3 with the mass ratio that dissolves and washes away agent, polyester slice and water and the ratio that dissolves and washes away agent, solid-to-liquid ratio is 1:5.
(4) spinning main technologic parameters:
A. polyester POY yarn spinning technique;
Spinning temperature: 280 DEG C;
Chilling temperature: 18 DEG C;
Winding speed: 3200m/min;
B. polyester FDY yarn spinning technique:
Spinning temperature: 280 DEG C;
Chilling temperature: 20 DEG C;
Network pressure: 0.20Mpa;
One roller speed: 2200m/min;
One roll temperature: 75 DEG C;
Two roller speed: 3600m/min;
Two roll temperatures: 115 DEG C;
Winding speed: 3600m/min;
C. composite filament processing technology:
Spin fast 400m/min;
Sizing over feed rate(OFR) 3.5%;
Coiling over feed rate(OFR) 2.5;
T1：180℃；
T2：150℃；
DR：1.6；
D/Y:1.6；
Network pressure: 0.05mpa.
The fracture strength 2.2cN/dtex that makes low aberration polyester Wool-Like abnormal contraction composite filament, elongation at break is 13.5%, curlingShrinkage factor is 8.50%, and network degree is 95/m, fiber number: 150dtex; The line of low aberration polyester Wool-Like abnormal contraction composite filament is closeDegree deviation ratio+2.5%, fracture strength CV value is 5.0%, and extension at break CV value is 10.0%, and boiling water shrinkage is 5.5%,Crimp contraction coefficient of variation CV value 9.6%, oil content is 1.1%; The line density deviation ratio 0.1% of low aberration polyester POY silk,Fracture strength 2.6cN/dtex, fracture strength CV value 2.8%, elongation at break is 80.0%, extension at break CV value 5.8%;The line density deviation ratio 0.43% of low aberration polyester FDY silk, fracture strength 4.6cN/dtex, fracture strength CV value 4.6%, disconnectedSplitting percentage elongation is 35%, extension at break CV value 9.3%, yarn unevenness CV1.93%, boiling water shrinkage 7.1%, oil content0.75％。
(5) dyeing
Embodiment 2
A preparation method for low aberration polyester Wool-Like abnormal contraction composite filament, main technique comprises:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite;Logical direct current, starting voltage 10V, cathode-current density is 200mA, electrolysis 12 hours 60 DEG C time, gets after electrolysis finishesGo out electrode, obtain white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol magnesium after being dried;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Esterification:
Adopt terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 2.0:1, adds anti-Ether agent calcium acetate, calcium acetate consumption is 0.05% of terephthalic acid (TPA) weight, carries out esterification after being made into uniform sizing material,To esterification products; Esterification is pressurizeed in nitrogen atmosphere, and pressure is controlled at 0.3MPa, and temperature is at 260 DEG C, and esterification water heats up in a steamerIt is esterification terminal that output reaches 92% of theoretical value;
Polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the polycondensation reaction low vacuum stage, add catalyst and stabilizing agent trimethyl phosphate in esterification products, and catalyst amount is0.05% of terephthalic acid (TPA) quality, trimethyl phosphate consumption is 0.05% of terephthalic acid (TPA) weight, under the condition of negative pressureStart polycondensation reaction, this staged pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature is controlled at 270 DEG C, when reactionBetween be 50 minutes; Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, and ethylene glycol magnesium and antimony glycol mass ratio are 3:1;
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, and reaction pressure is down to definitelyPressure 95Pa, reaction temperature is controlled at 280 DEG C, 90 minutes reaction time; Make polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent propyl cellosolve 130 DEG C with 0.3MPa condition under brew 5 hours, by washingWash, i.e. 80 DEG C of hot water wash 15min for polyester slice after brew, then clean with cold water, and Drying and cooling is for subsequent use; GatheredEster, water is 100:4 with the mass ratio that dissolves and washes away agent, polyester slice and water and the ratio that dissolves and washes away agent, solid-to-liquid ratio is 1:10.
(4) spinning main technologic parameters:
A. polyester POY yarn spinning technique;
Spinning temperature: 290 DEG C;
Chilling temperature: 22 DEG C;
Winding speed: 3600m/min;
B. polyester FDY yarn spinning technique:
Spinning temperature: 290 DEG C;
Chilling temperature: 25 DEG C;
Network pressure: 0.30Mpa;
One roller speed: 2600m/min;
One roll temperature: 85 DEG C;
Two roller speed: 3900m/min;
Two roll temperatures: 135 DEG C;
Winding speed: 3800m/min;
C. composite filament processing technology:
Spin fast 800m/min;
Sizing over feed rate(OFR) 5.50%;
Coiling over feed rate(OFR) 5.0;
T1：220℃；
T2：180℃；
DR：1.8；
D/Y:2.0；
Network pressure: 0.3mpa.
The fracture strength 2.5cN/dtex that makes low aberration polyester Wool-Like abnormal contraction composite filament, elongation at break is 13.0%, curlingShrinkage factor is 2.5%, and network degree is 85/m, fiber number: 300dtex; The line of low aberration polyester Wool-Like abnormal contraction composite filament is closeDegree deviation ratio 2.3%, fracture strength CV value 4.9%, extension at break CV value 9.4%, boiling water shrinkage is 5.5%, curling receiptsShrinkage coefficient of variation CV value 9.8%, oil content is-0.1%; The line density deviation ratio 0.15% of low aberration polyester POY silk, disconnectedResistance to spalling 3.2cN/dtex, fracture strength CV value 2.6%, elongation at break is 96%, extension at break CV value 5.3%. ; LowThe line density deviation ratio 0.43% of aberration polyester FDY silk, fracture strength 4.1cN/dtex, fracture strength CV value 4.6%, fracturePercentage elongation is 34.0%, extension at break CV value 8.9%, yarn unevenness CV1.85%, boiling water shrinkage 7.7%, oil content1.05％。
(5) dyeing
Embodiment 3
A preparation method for low aberration polyester Wool-Like abnormal contraction composite filament, main technique comprises:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite;Logical direct current, starting voltage 7V, cathode-current density is 160mA, electrolysis 11 hours 55 DEG C time, gets after electrolysis finishesGo out electrode, obtain white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol magnesium after being dried;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Esterification:
Adopt terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 1.5:1, adds anti-Ether agent sodium acetate, sodium acetate consumption is 0.02% of terephthalic acid (TPA) weight, carries out esterification after being made into uniform sizing material,To esterification products; Esterification is pressurizeed in nitrogen atmosphere, and pressure is controlled at 0.2MPa, and temperature is at 255 DEG C, and esterification water heats up in a steamerIt is esterification terminal that output reaches 92% of theoretical value;
Polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the polycondensation reaction low vacuum stage, in esterification products, add catalyst and stabilizing agent Trimethyl phosphite, catalyst amountFor 0.02% of terephthalic acid (TPA) quality, Trimethyl phosphite consumption is 0.02% of terephthalic acid (TPA) weight, at the bar of negative pressureUnder part, start polycondensation reaction, this staged pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature is controlled at 265 DEG C, anti-Between seasonable, it is 35 minutes; Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium and antimony glycol mass ratioFor 3:1;
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, and reaction pressure is down to definitelyPressure 98Pa, reaction temperature is controlled at 277 DEG C, 60 minutes reaction time; Make polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent ethylene glycol monobutyl ether (EGMBE) 125 DEG C with 0.2MPa condition under brew 3 hours, by washingWash, i.e. 70 DEG C of hot water wash 15min for polyester slice after brew, then clean with cold water, and Drying and cooling is for subsequent use; GatheredEster, water is 100:4 with the mass ratio that dissolves and washes away agent, polyester slice and water and the ratio that dissolves and washes away agent, solid-to-liquid ratio is 1:10.
(4) spinning main technologic parameters:
A. polyester POY yarn spinning technique;
Spinning temperature: 285 DEG C;
Chilling temperature: 20 DEG C;
Winding speed: 3500m/min;
B. polyester FDY yarn spinning technique:
Spinning temperature: 285 DEG C;
Chilling temperature: 22 DEG C;
Network pressure: 0.25Mpa;
One roller speed: 2500m/min;
One roll temperature: 78 DEG C;
Two roller speed: 3800m/min;
Two roll temperatures: 120 DEG C;
Winding speed: 3700m/min;
C. composite filament processing technology:
Spin fast 500m/min;
Sizing over feed rate(OFR) 5.0%;
Coiling over feed rate(OFR) 3.5;
T1：200℃；
T2：170℃；
DR：1.7；
D/Y:1.7；
Network pressure: 0.25mpa.
The fracture strength 2.9cN/dtex that makes low aberration polyester Wool-Like abnormal contraction composite filament, elongation at break is 13.5%, curlingShrinkage factor is 3.5%, and network degree is 94/m, fiber number: 250dtex; The line of low aberration polyester Wool-Like abnormal contraction composite filament is closeDegree deviation ratio-2.3%, fracture strength CV value is 4.3%, extension at break CV value 9.6%, boiling water shrinkage is 4.5%, curlingShrinkage factor coefficient of variation CV value 9.2%, oil content is 1.1%; The line density deviation ratio 0.15% of low aberration polyester POY silk,Fracture strength 3.4cN/dtex, fracture strength CV value 2.6%, elongation at break is 100%, extension at break CV value 5.3%;The line density deviation ratio 0.36% of low aberration polyester FDY silk, fracture strength 4.6cN/dtex, fracture strength CV value 3.9%, disconnectedSplitting percentage elongation is 32%, extension at break CV value 9.2%, yarn unevenness CV1.96%, boiling water shrinkage 7.6%, oil content0.96％。
(5) dyeing
Embodiment 4
A preparation method for low aberration polyester Wool-Like abnormal contraction composite filament, main technique comprises:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite;Logical direct current, starting voltage 7V, cathode-current density is 170mA, electrolysis 11 hours 58 DEG C time, gets after electrolysis finishesGo out electrode, obtain white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol magnesium after being dried;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Esterification:
Adopt terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and described terephthalic acid (TPA) is 1.8:1, addsEnter anti-ether agent sodium acetate, sodium acetate consumption is 0.02% of terephthalic acid (TPA) weight, carries out esterification after being made into uniform sizing material,Obtain esterification products; Esterification is pressurizeed in nitrogen atmosphere, and pressure is controlled at 0.3MPa, and temperature is at 250 DEG C, esterification waterIt is esterification terminal that quantity of distillate reaches 98% of theoretical value;
Polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the polycondensation reaction low vacuum stage, add catalyst and stabilizing agent triphenyl phosphate in esterification products, and catalyst amount is0.02% of described terephthalic acid (TPA) quality, triphenyl phosphate consumption is 0.02% of terephthalic acid (TPA) weight, at the bar of negative pressureUnder part, start polycondensation reaction, this staged pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature is controlled at 264 DEG C, anti-Between seasonable, it is 38 minutes; Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium and antimony glycol mass ratioFor 3:1;
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, and reaction pressure is down to definitelyPressure 99Pa, reaction temperature is controlled at 280 DEG C, 90 minutes reaction time; Make polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent ethylene glycol monoethyl ether 120 DEG C with 0.3MPa condition under brew 3 hours, by washingWash, i.e. 70 DEG C of hot water wash 15min for polyester slice after brew, then clean with cold water, and Drying and cooling is for subsequent use; GatheredEster, water is 100:4 with the mass ratio that dissolves and washes away agent, polyester slice and water and the ratio that dissolves and washes away agent, solid-to-liquid ratio is 1:8.
(4) spinning main technologic parameters:
A. polyester POY yarn spinning technique;
Spinning temperature: 282 DEG C;
Chilling temperature: 20 DEG C;
Winding speed: 3500m/min;
B. polyester FDY yarn spinning technique:
Spinning temperature: 285 DEG C;
Chilling temperature: 23 DEG C;
Network pressure: 0.25Mpa;
One roller speed: 2300m/min;
One roll temperature: 82 DEG C;
Two roller speed: 3800m/min;
Two roll temperatures: 125 DEG C;
Winding speed: 3650m/min;
C. composite filament processing technology:
Spin fast 600m/min;
Sizing over feed rate(OFR) 4.5%;
Coiling over feed rate(OFR) 4.0;
T1：190℃；
T2：150-℃；
DR：1.8；
D/Y:2.0；
Network pressure: 0.05mpa.
The fracture strength 2.6cN/dtex that makes low aberration polyester Wool-Like abnormal contraction composite filament, elongation at break is 14.2%, curlingShrinkage factor is 2.6%, and network degree is 86/m, fiber number: 180dtex; The line of low aberration polyester Wool-Like abnormal contraction composite filament is closeDegree deviation ratio+2.3%, fracture strength CV value 3.9%, extension at break CV value 9.2%, boiling water shrinkage is 4.2%, curling receiptsShrinkage coefficient of variation CV value 9.3%, oil content is 1.0%; The line density deviation ratio 0.1% of low aberration polyester POY silk, fractureIntensity 2.9cN/dtex, fracture strength CV value 2.6%, elongation at break is 98%, extension at break CV value 5.3%; Low aberrationThe line density deviation ratio 0.36% of polyester FDY silk, fracture strength 4.5cN/dtex, fracture strength CV value 3.9%, extension at breakRate is 35%, extension at break CV value 9.1%, yarn unevenness CV1.96%, boiling water shrinkage 7.8%, oil content 0.85%.
(5) dyeing
Claims (10)
1. a low aberration polyester Wool-Like abnormal contraction composite filament, is characterized in that: described low aberration Wool-Like abnormal contraction composite filament is low lookPoor polyester POY silk and low aberration polyester FDY silk are through the composite filament of mixed fine processing composition, described low aberration polyester POY silkForming tiny wire ring is centered around around described low aberration polyester FDY silk; Described low aberration polyester POY silk and low aberration polyesterFDY silk is via polyester spinning and obtain the fracture strength of described low aberration polyester Wool-Like abnormal contraction composite filament after dissolveing and washing away>=2.1cN/dtex, elongation at break is 15.0 ± 2.0%, and crimp contraction is 5.50 ± 3.0%, and network degree is 90 ± 5/m,Fiber number: 150-300dtex; Aberration Δ E is less than 0.200; Described polyester is that terephthalic acid (TPA) and ethylene glycol are through esterification with in secondPolycondensation under the mixture through catalytic effect of two magnesium alkoxides and antimony glycol, then obtain polyester slice through pelletizing;
Described industry is with in the section of polyester, and oligomer mass percentage content is less than 0.5%, the mass percent of diethylene glycol (DEG)Content is less than 0.5%;
The molecular formula of described ethylene glycol magnesium is Mg (OCH2CH2OH)2；
Described dissolve and wash away the section that refers to after granulation through water with dissolve and wash away agent 120～130 DEG C with 0.2～0.3MPa condition under brew andWashing.
2. the low aberration polyester of one according to claim 1 Wool-Like abnormal contraction composite filament, is characterized in that, described low aberration is poly-Line density deviation ratio ± 2.5% of ester Wool-Like abnormal contraction composite filament, fracture strength CV value≤5.0%, extension at break CV value≤ 10.0%, boiling water shrinkage is 5.0 ± 1.0%, crimp contraction coefficient of variation CV value≤10.0%, and oil content is 1.0 ± 0.2%;Line density deviation ratio≤0.2% of low aberration polyester POY silk, fracture strength >=2.6cN/dtex, fracture strength CV value≤3.0%,Elongation at break is 90.0 ± 10.0%, extension at break CV value≤6.0%. ; The line density deviation ratio of low aberration polyester FDY silk≤ 0.5%, fracture strength >=3.8cN/dtex, fracture strength CV value≤5.0%, elongation at break is 33.0 ± 3.0%, fracture is stretchedLong CV value≤10.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 0.90 ± 0.20%.
3. the low aberration polyester of one according to claim 1 Wool-Like abnormal contraction composite filament, is characterized in that, described ethylene glycol magnesiumIn the mixture of antimony glycol, ethylene glycol magnesium and antimony glycol mass ratio are 2～3:1.
4. the preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament as described in any one in claim 1～3, its featureBe: by polyester through measuring, extrude, cooling, oil and reel, make low aberration modified poly ester POY silk; Cut by polyesterSheet through measuring, extrude, cooling, oil, stretching, thermal finalization and coiling, make low aberration polyester FDY silk; Then willLow aberration polyester POY silk and low aberration polyester FDY silk through plying network, add hot-stretch, false twisting, thermal finalization and be wound intoType makes low aberration polyester Wool-Like abnormal contraction composite filament.
5. according to the preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament of claim 4, it is characterized in that main workSkill comprises:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite;Logical direct current, starting voltage 6～10V, cathode-current density is 150～200mA, electrolysis 10～12 hours 50～60 DEG C time,Electrolysis finishes rear taking-up electrode, obtains white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtains after being driedEthylene glycol magnesium;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt terephthalic acid (TPA) and ethylene glycol as raw material, add anti-ether agent, carry out esterification after being made into uniform sizing material,To esterification products; Esterification is pressurizeed in nitrogen atmosphere, and pressure is controlled at normal pressure～0.3MPa, and temperature is at 250～260 DEG C,What esterification water quantity of distillate reached theoretical value more than 90% is esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction low vacuum stage, add catalyst and stabilizing agent in esterification products, under the condition of negative pressure, startsPolycondensation reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature is controlled at 260～270 DEG C, anti-Between seasonable, it is 30～50 minutes; Described catalyst is the mixture of ethylene glycol magnesium and antimony glycol;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and makes reaction pressureBe down to absolute pressure and be less than 100Pa, reaction temperature is controlled at 275～280 DEG C, 50～90 minutes reaction time;
Make polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Described polyester slice through water with dissolve and wash away agent 120～130 DEG C with 0.2～0.3MPa condition under brew 3-5 hour, by washingWash; Obtain polyester;
(4) spinning processing main technologic parameters:
A. polyester POY yarn spinning technique;
Spinning temperature: 280-290 DEG C;
Chilling temperature: 18-22 DEG C;
Winding speed: 3200-3600m/min;
B. polyester FDY yarn spinning technique:
Spinning temperature: 280-290 DEG C;
Chilling temperature: 20-25 DEG C;
Network pressure: 0.20-0.30Mpa;
One roller speed: 2200-2600m/min;
One roll temperature: 75-85 DEG C;
Two roller speed: 3600-3900m/min;
Two roll temperatures: 115-135 DEG C;
Winding speed: 3600-3800m/min;
C. composite filament processing technology:
Spin fast 400-800m/min;
Sizing over feed rate(OFR) 3.5-5.50%;
Coiling over feed rate(OFR) 2.5-5.0;
T1：180-220℃；
T2：150-180℃；
DR：1.6-1.8；
D/Y:1.6-2.0；
Network pressure: 0.05-0.3mpa.
6. according to the preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament described in claim 4 or 5, it is characterized in that,The mol ratio of described ethylene glycol and described terephthalic acid (TPA) is 1.2～2.0:1.
7. the preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament according to claim 5, is characterized in that instituteState in the mixture of ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium and antimony glycol mass ratio are 2～3:1; Described catalyst is usedAmount is 0.01%～0.05% of described terephthalic acid (TPA) quality; Described stabilizing agent is selected from triphenyl phosphate, trimethyl phosphate and AsiaOne in trimethyl phosphate, stabilizing agent dosage is 0.01%～0.05% of described terephthalic acid (TPA) weight.
8. the preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament according to claim 5, is characterized in that instituteStating water is 100:3～4 with the mass ratio that dissolves and washes away agent, polyester slice and water and the ratio that dissolves and washes away agent, and solid-to-liquid ratio is 1:5～10;It is described that to dissolve and wash away agent be the one in ethylene glycol monoethyl ether, propyl cellosolve and ethylene glycol monobutyl ether (EGMBE).
9. the preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament according to claim 5, is characterized in that instituteState washing and refer to after brew 70～80 DEG C of hot water wash 10～15min polyester slice for, then clean with cold water, Drying and cooling is standbyWith.
10. the preparation method of a kind of low aberration polyester Wool-Like abnormal contraction composite filament according to claim 5, is characterized in that,Described anti-ether agent is the one in sodium acetate and calcium acetate, and anti-ether agent consumption is described terephthalic acid (TPA) weight0.01％～0.05％。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511018915.6A CN105648570B (en) | 2015-12-29 | 2015-12-29 | A kind of low aberration polyester Wool-Like abnormal contraction composite filament and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511018915.6A CN105648570B (en) | 2015-12-29 | 2015-12-29 | A kind of low aberration polyester Wool-Like abnormal contraction composite filament and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105648570A true CN105648570A (en) | 2016-06-08 |
| CN105648570B CN105648570B (en) | 2017-12-15 |
Family
ID=56477434
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511018915.6A Active CN105648570B (en) | 2015-12-29 | 2015-12-29 | A kind of low aberration polyester Wool-Like abnormal contraction composite filament and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105648570B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107604464A (en) * | 2017-09-07 | 2018-01-19 | 江苏恒科新材料有限公司 | A kind of preparation method of double odd-shaped cross section moisture absorbing and sweat releasing fiber types |
| JP2019515153A (en) * | 2016-08-31 | 2019-06-06 | 江蘇恒力化繊股▲ふん▼有限公司 | Hetero-shrinkage mixed fiber and method for producing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594660A (en) * | 2004-07-05 | 2005-03-16 | 苏州大学 | Process for synthesizing glycol antimony |
| CN104480567A (en) * | 2014-12-31 | 2015-04-01 | 江苏恒力化纤股份有限公司 | Wool-like differential shrinkage composite filament and preparation method thereof |
| CN104878487A (en) * | 2014-12-31 | 2015-09-02 | 江苏恒力化纤股份有限公司 | Composite differential shrinkage yarn and preparation method thereof |
-
2015
- 2015-12-29 CN CN201511018915.6A patent/CN105648570B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594660A (en) * | 2004-07-05 | 2005-03-16 | 苏州大学 | Process for synthesizing glycol antimony |
| CN104480567A (en) * | 2014-12-31 | 2015-04-01 | 江苏恒力化纤股份有限公司 | Wool-like differential shrinkage composite filament and preparation method thereof |
| CN104878487A (en) * | 2014-12-31 | 2015-09-02 | 江苏恒力化纤股份有限公司 | Composite differential shrinkage yarn and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 冯新德等: "《饱和聚酯与缩聚反应》", 28 February 1986, 科学出版社 * |
| 魏家瑞等: "《热塑性聚酯及其应用》", 31 January 2012, 化学工业出版社 * |
| 魏文良: ""聚酯中齐聚物的表征及控制方法研究"", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019515153A (en) * | 2016-08-31 | 2019-06-06 | 江蘇恒力化繊股▲ふん▼有限公司 | Hetero-shrinkage mixed fiber and method for producing |
| EP3508625A4 (en) * | 2016-08-31 | 2019-09-18 | Jiangsu Hengli Chemical Fibre Co., Ltd. | Different-shrinkage composite yarn and preparation method therefor |
| CN107604464A (en) * | 2017-09-07 | 2018-01-19 | 江苏恒科新材料有限公司 | A kind of preparation method of double odd-shaped cross section moisture absorbing and sweat releasing fiber types |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105648570B (en) | 2017-12-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105671675B (en) | A kind of low aberration polyester imitates cotton abnormal contraction composite filament and preparation method thereof | |
| CN104480567B (en) | A kind of Wool-Like abnormal contraction composite filament and preparation method thereof | |
| CN104480568B (en) | A kind of imitative linen look abnormal contraction composite filament and preparation method thereof | |
| CN105442082B (en) | A kind of low aberration polyester HOY silks and preparation method thereof | |
| CN105463619B (en) | A kind of low aberration polyester POY silks and preparation method thereof | |
| CN104562340A (en) | Differential-shrinkage cotton-like composite filament and preparation method thereof | |
| CN105648571B (en) | A kind of low aberration polyester DTY silks and preparation method thereof | |
| CN105586660A (en) | A production method for hydrophilic moisture-transmitting polyester staple fibers specially used for vortex spinning | |
| CN106400168B (en) | Porous super soft imitative cotton polyester fiber of one kind and preparation method thereof | |
| CN101570596B (en) | Method for preparing cationic-dyeable copolyester | |
| CN103467716B (en) | Disperse dye normal pressure engrain copolyether ester and ultra-fine fibre thereof | |
| CN102080285B (en) | Production method of spunbonded polyester embroidery thread and product of same | |
| CN105648594B (en) | A kind of low aberration polyester imitates linen look abnormal contraction composite filament and preparation method thereof | |
| CN105506774B (en) | A kind of low aberration polyester abnormal contraction composite filament and preparation method thereof | |
| CN105648570A (en) | Low-color-difference polyester wool-like different-shrinkage complex yarn and preparation method thereof | |
| CN106592001B (en) | A kind of aromatic polyester-aliphatic polyester block copolymerization ester fiber and purposes | |
| CN106319679B (en) | Porous soft imitative hair polyester fiber of one kind and preparation method thereof | |
| CN106400170B (en) | Porous super soft imitative numb polyester fiber of one kind and preparation method thereof | |
| CN105646857B (en) | A kind of leaf shaped filaments of low aberration polyester superbright light three and preparation method thereof | |
| CN105506775B (en) | A kind of super soft ultrafine wire of low aberration polyester and preparation method thereof | |
| CN106835437B (en) | A kind of aromatic polyester-aliphatic polyester block copolymerization ester fiber and protein fibre fabric | |
| CN105463618B (en) | A kind of low aberration polyester DTY light silks and preparation method thereof | |
| CN206051915U (en) | A kind of preparation facilitiess of colorful intelligent digital yarn | |
| CN105648566B (en) | A kind of low aberration polyester FDY silks and preparation method thereof | |
| CN106381550B (en) | Porous soft imitative cotton polyester fiber of one kind and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |