CN102051706B - Copolyester false-twist yarn and production method thereof - Google Patents

Copolyester false-twist yarn and production method thereof Download PDF

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Publication number
CN102051706B
CN102051706B CN200910174448.4A CN200910174448A CN102051706B CN 102051706 B CN102051706 B CN 102051706B CN 200910174448 A CN200910174448 A CN 200910174448A CN 102051706 B CN102051706 B CN 102051706B
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China
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false
copolyester
twist yarn
fiber
polyester
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CN102051706A (en
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冯杨梅
清水敏昭
景红川
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Toray Industries Inc
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Toray Fibers and Textiles Research Laboratories China Co Ltd
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Abstract

The invention discloses a copolyester false-twist yarn and a production method thereof. The false-twist yarn comprises at least one component, namely copolyester fibers containing a 2-mhyl-1,3-popanediol structure, and the copolyester fibers containing the 2-mhyl-1,3-popanediol structure accounts for 20 to 100 weight percent of the whole copolyester false-twist yarn. The copolyester false-twist yarn has the filament number of 0.01 to 10dtex, the breaking strength of 1.5 to 5cN/dtex and the elongation at break of 15 to 40 percent. The false-twist yarn can be dyed by a disperse dye at normal temperature and normal pressure, and the color emissivity at normal temperature and normal pressure is close to or reaches the color emissivity of the non-modified polyester at high temperature under high pressure. The invention can be widely applied to the fields such as clothing, decoration and industry.

Description

A kind of copolyester false-twist yarn and production method thereof
Technical field
The present invention relates to a kind of copolyester false-twist yarn and production method thereof, more particularly relate to a kind of normal pressure dyeable copolyester false twist yarn, belong to synthetic fiber field.
Background technology
Polyester fiber, owing to having excellent properties, has been obtained the development attracting people's attention since large-scale production.
And along with technical development, when polyester fiber quantitatively constantly satisfies social needs, in the improvement of also carrying out qualitatively hommization more.Aspect improvement feel, people make polyester have the more feel of comfortable by means such as special-shaped section, copolymerization, composit false twisting processing, aspect modify appearance, people, by special processing method, make cloth cover present ombre effect or thickness joint stripe effect etc.But aspect the dyeability of raising polyester, remaining a very difficult problem, as everyone knows, polyester fiber is due to architectural characteristic closely between macromolecular chain, can only under High Temperature High Pressure, dye, not only environmental protection and energy-conservation on existing problems and to dyeing installation and technological requirement harshness, cost is also higher.At present, improving dying polymers performance by combined polymerization technology is one of main means, for example: with the polymer forming after the straight chain such as polymer or adipic acid, the decanedioic acid aliphatic carboxylic acid copolymerization forming after the poly alkylene glycol copolymerization of polyethylene glycol and so on.But these methods must add ehter bond or many monomer copolymerizables, so also will cause heat resistance to decline.Also the structure of taking dyeing assistant or changing dyestuff having is to realize the dyeing under polyester low-temperature condition, but actual effect not obvious.
In patent CN101063236A, CN1534114A, disclose by forming the method for polyester with dihydroxylic alcohols copolymerization with side chain.But the heat resistance of these polyester is still bad, cause the problems such as the physical property of spinning difficulty or fiber is bad.
Summary of the invention
The object of the present invention is to provide copolyester false-twist yarn and the production method thereof of the normal-temperature normal-pressure dyeable that a kind of dyeability is good, heat resistance is high, dyefastness is good.
Technical solution of the present invention is:
In this copolyester false-twist yarn, at least one is containing 2-methyl isophthalic acid, the copolyester fiber of ammediol structure, and it is containing 2-methyl isophthalic acid, and the percentage by weight that the copolyester fiber of ammediol structure accounts for whole copolyester false-twist yarn is 20~100%.
Containing 2-methyl isophthalic acid, when the copolyester fiber of ammediol structure and other fiber composite, consider the condition of cost and low temperature dyeing, other fiber can be nylon fiber, cellulose fibre or cationic fiber, and the percentage by weight that other fiber accounts for whole copolyester false-twist yarn is 0~80%.Containing 2-methyl isophthalic acid, the copolyester fiber of ammediol structure is particularly suitable for carrying out composit false twisting processing with needs low temperature dyeing fiber.
Forming should be containing 2-methyl isophthalic acid, and the content of the terminal carboxyl group COOH of the polyester in the copolyester false-twist yarn of ammediol structure is below 25 equivalents/ton, if when the content of terminal carboxyl group is greater than 25 equivalents/ton, will make the heat resistance of copolyesters reduce; Preferably below 20 equivalents/ton.In polyester, the content of diethylene glycol (DEG) is below 2.0wt%, and now the heat resistance of copolymer is very good.Diethylene glycol (DEG) is secondaryly in the time that polyester is synthetic rawly to form and exist with the form of closing with polyethylene terephthalate copolymer, when the content of diethylene glycol (DEG) exceedes 2.0wt%, when spinning, the temperature of the fusing point of polyester or beginning melting is low, can cause that heat resistance declines, degradation problem under the feel of the finished product being made into by this fiber.Preferably diethylene glycol (DEG) content is below 1.5wt%.In carrying out polymerisation rapidly, also to keep the high-fire resistance of polyester, so the phosphorus atoms content P in polyester of the present invention and metallic atom content M meet formula (1) and formula (2):
5≤[P]≤100 (ppm) formulas (1)
0.1≤[M]/[P]≤30 formulas (2).
The content of phosphorus atoms is less than 5ppm, while being greater than 100ppm, the heat resistance of copolyesters is bad, and polymerisation can not be carried out smoothly thereby formation efficiency is low.
And the ratio of the content P of metallic atom content M and phosphorus atoms is less than 0.1, is greater than at 30 o'clock, when polymerisation is difficult to carry out productivity ratio reduction, the heat resistance of the polymer obtaining is not good; Preferably 1≤[M]/[P]≤15.
The filament number of false twist yarn is 0.01~10dtex, and fracture strength is 1.5~5cN/dtex, and elongation at break is 15~40%.
The L value A that false twist yarn adopts DISPERSE DYES to dye under the condition of the normal temperature and pressure of 90~100 ℃, the L value B after the normal polyester fiber suitable with single fiber quantity with fiber number dyes under 130 ℃ of conditions compares, and meets formula (3):
-8 < (A-B) < 10 formulas (3).
The production method of copolyester false-twist yarn of the present invention is as follows:
(1) select the methyl isophthalic acid containing 2-, the polyester slice of ammediol structure, makes copolyesters pre-oriented yarn or extends silk;
(2) the copolyesters pre-oriented yarn of step (1) gained or extension silk are directly carried out to drafting false twisting processing; Or carry out composite drafting false twisting processing with other fibers, obtain product, according to purposes and required, make single false twisting false twist yarn or composit false twisting false twist yarn, its false twisting processing conditions is as follows: drawing-off multiplying power is 1.0~1.8, and this drawing-off multiplying power is total draft multiplying power, can be divided into interior drawing-off and outer drawing-off.Total draft multiplying power is below 1.0 time, and false twist yarn can not obtain enough maintenance tension force, and to cause processing stability not good; Drawing-off multiplying power is 1.8 when above, and false twist yarn is excessively stretched, and can cause false twist yarn to produce filoplume and cause intensity significantly to reduce.The wherein preferred nylon fiber of other fibers, cellulose fibre or cationic fiber.
It is the hot case of contact of 140~250 ℃ or to adopt temperature be the contactless hot case of 280~600 ℃ that the first hot case adopts temperature; Contact heater temperature is below 140 ℃ or contactless heater temperature below 280 ℃ time, and false twist yarn can not obtain good fixed effect, causes processing stability poor; Contact heater temperature is in the time that 250 ℃ or contactless heater temperature are more than 600 ℃, and false twist yarn is molten and can causes false twist yarn intensity extremely low and can not meet the tension force requirement of later process.It is 100~230 ℃ of hot casees of contact that the second hot case also can be selected temperature, or to select temperature be 280~600 ℃ of contactless hot casees.
The filament number of the copolyester false-twist yarn that the method makes is 0.01~10dtex, and fracture strength is 1.5~5cN/dtex, and elongation at break is 15~40%.This false twist yarn can dye at normal temperatures and pressures, adopts DISPERSE DYES, when dyeing temperature is 90~100 ℃, with 130 ℃ of dyeing without compared with the polyester of upgrading, color emissivity is good, dyefastness is high.Dyeing at normal temperatures and pressures has superiority in energy-conservation and purposes, can be widely used in garment industry, decoration field and industrial field.
The specific embodiment
Below by embodiment, the present invention will be described in more detail.In addition, the each physics value in embodiment and comparative example is measured by following methods.
(1) the intrinsic viscosity IV of polymer
Measure at 25 ℃ using o-chlorphenol as solvent.
(2) the terminal carboxyl group COOH (equivalent/ton) in polymer
Using o-cresol as solvent, the NaOH aqueous solution with concentration 0.02mol/L at 25 ℃ is measured on automatic titration device (COM-550 that Ping Zhao industry company produces).
(3) content of diethylene glycol (DEG) (wt%) in polymer
Using monoethanolamine as solvent, heating for dissolving after mixing with 1,6-ethylene glycol/methyl alcohol, then adds methyl alcohol ultrasonic cleaner to clean 10min.Then add acid to carry out neutralisation treatment, after filtration, use gas chromatograph (Shimadzu Seisakusho Ltd. produces GC-14A) to measure filtrate.
(4) tenor in polymer
6g polymer is pressed into sheet, measures its intensity with fluorescent x-ray analysis apparatus (of science electric corporation manufacture x-ray analysis device 3270 types), convert with the detection line that the sample of known metal content makes in advance.
(5) false twist yarn fiber number
By the test of GB GB/T 14343-2003B method
(6) false twist yarn fracture strength
Use the Tensilon instrument of Japanese AND company to measure, upper and lower jaws distance is set as 20cm, and draw speed is set as 200mm/min, and initial tension is set as: Den*0.1g, requires to insert the data such as fiber number according to menu.After setting check is good, start to stretch, automatically draw yarn breakage intensity data.
(7) false twist yarn elongation at break
Use the Tensilon instrument of Japanese AND company to measure, upper and lower jaws distance is set as 20cm, and draw speed is set as 200mm/min, and initial tension is set as: Den*0.1g, requires to insert the data such as fiber number according to menu.After setting check is good, start to stretch, automatically show that yarn breakage extends data.
(8) L value
Sample is overlapped into after light tight shape with spectral photometric colour measuring meter (Datacolor 650 that Datacolor AsiaPacific (H.K.) Ltd. manufactures) colour examining, automatically draws L value.L refers to the lightness of L*a*b* color specification system, and the less dyeability of numerical value is better.
(9) color fastness to light
Test by JISL0842 the 4th exposure method
(10) washing fastness
Test by JISL0844A-2 method
[embodiment 1]
Bishydroxyethyl terephthalate is added to esterification groove, keep 250 ℃ of temperature, pressure 1.2 × 10 5pa joined gradually esterification layer by the ethylene glycol slurry of the high purity terephthalic acid of 8.25kg and 3.54kg in 4 hours, then carried out the esterification of 1 hour.Finally from the reactant of esterification obtaining, get 10.2kg and join polycondensation reaction layer.
Esterification reaction product is remained under 250 ℃, normal pressure, add and be equivalent in gained polyester all 2-methyl isophthalic acids of dihydroxylic alcohols 10mol% amount, 3 propylene glycol carry out the stirring of 30min.Then add phosphorus atoms amount to be equivalent to the phosphoric acid of the 18ppm of polymer, after 5min, add antimony atoms amount to be equivalent to the antimonous oxide of polymer 230ppm, and cobalt atom amount is equivalent to the cobalt acetate of polymer 15ppm.After 5min, add Titanium particles amount to be equivalent to the ethylene glycol slurry containing Titanium particles of polymer 0.3wt%.After 5min, start decompression, heat up.Temperature rises to 290 ℃, Pressure Drop to 40Pa by 250 ℃.After 90min, reach final temperature, final pressure.Arrive after certain stirring extent, be back to normal pressure to importing nitrogen in reaction system, stop polycondensation reaction.Polymer is strip and spues, cooling rear section in tank.
The content that the intrinsic viscosity of resulting polymers is 0.67, the concentration of terminal groups COOH is 19 equivalents/ton, DEG is that the content of 0.95wt%, phosphorus atoms is that the content of 18ppm, cobalt atom is that the content of 15ppm, antimony atoms is that the content of 230ppm ([M]/[P]=3.7), Titanium particles is 0.3wt%.
Make its moisture rate remain on 50ppm the chip drying obtaining, then melt spinning under the spinning temperature of 290 ℃, under the hauling speed of 3000m, batch, make the pre-oriented yarn of 90dtex/24f. on false twist apparatus, be 1.7 by drawing-off multiplying power, process velocity is 500m/min, the first hot case employing temperature is the hot case of contact of 190 ℃, the second heater temperature is that to obtain fiber number be 54dtex in the condition processing of the hot case of contact of 170 ℃, fracture strength is 3.5cN/dtex, the false twist yarn that elongation at break is 28%.The false twist yarn obtaining is carried out to cylinder to be compiled, and use refining agent 2g/L, NaOH 2g/l, 95 ℃ of * 15min, carry out refining processing with water-bath than 1: 20~50, after 170 ℃ of * 1min baking oven sizings, use URMINI-COLOR (the small-sized dyeing machine of infrared ray, TEXAM technical research is manufactured) to dye under the condition of 95 ℃ × 30min.Dye well auxiliary agent is as follows:
Dianix Blue E-Plus (manufacture of De Sida company, DISPERSE DYES)
0.3owf% and 5owf%
NIKKA SUNSALT (manufacture of solar corona chemical company, levelling agent) 1g/l
Acetic acid (pH adjusting agent) 1g/l
After dyeing, the medicament below using under the condition of 80 ℃ × 20min carries out reduction cleaning.
NaOH 2g/l
Sodium hydrosulfite 2g/l
Then, by cylinder compile thing washing, air-dry after, measure cylinder and compile the L value of thing, when dyestuff 0.3owf%, L value A is 56, color fastness to light is more than 4 grades.When dyestuff 5owf%, L value A ' is 29, and washing fastness is more than 4 grades.
Also can clearly be seen that from comparative example below, with not and 2-methyl isophthalic acid, the polyethylene terephthalate of ammediol combined polymerization is compared, copolyester false-twist yarn of the present invention is (A-B)=2 after normal temperature and pressure dyeing, (A '-B ')=7, meet formula (3): the requirement of-8 < (A-B) < 10, the dyeability of the polyester false twist yarn that approaches common non-modified in the time of high-temp dyeing, dyeing at normal temperatures and pressures has splendid superiority in energy-conservation and purposes.
[comparative example 1]
Do not add 2-methyl isophthalic acid, ammediol, all the other conditions, with embodiment 1, obtain the polyester false twist yarn of common non-modified.Dyeing temperature is 130 ℃, and when dyestuff 0.3owf%, L value B is 54, and color fastness to light is more than 4 grades, and when dyestuff 5owf%, L value B ' is 22, and washing fastness is 4 grades.
The polyester false twist yarn of non-modified, under 95 ℃ of dyeing temperature conditions, when dyestuff 0.3owf%, L value is 61, and color fastness to light is 3~4 grades, and when dyestuff 5%, L value is 37, and washing fastness is 3~4 grades, color emissivity is bad.
[embodiment 2]
Select the copolyester section described in same embodiment 1, then melt spinning under the spinning temperature of 280 ℃, under the hauling speed of 3000m/min, batch, the undrawn yarn obtaining stretches under the condition of 90 ℃ of draft temperatures, 1.65 times of stretching ratios, then at 130 ℃, after HEAT SETTING, batch, obtain the extension silk A silk of 110dtex/24f.Its fiber number is 110dtex, and fracture strength is 4.3cN/dtex, and elongation at break is 31%.Select B yarn toray produce cellulose fibre (this fiber is under low temperature dyeing condition, the excellent performances such as intensity) preliminary draft silk and the A silk of Foresse fiber 90dtex/36f carry out composit false twisting processing, false twisting processing conditions is that outer drawing-off multiplying power is 0.995, interior drawing-off multiplying power is 1.02, first interlacing pneumatics is 0.4MPa, rear interlacing pneumatics is 0.2MPa, process velocity is 350m/min, the first hot case employing temperature is the contactless hot case of 390 ℃, obtaining fiber number is 200dtex, fracture strength is 2.3cN/dtex, the false twist yarn that elongation at break is 25%.Wherein to account for the percentage by weight of whole false twist yarn be 55% to A silk, the false twist yarn obtaining is carried out to cylinder by method described in embodiment 1 to be compiled, concise, sizing, dyeing, the processing such as reduction cleaning, dyestuff is Dianix Black ETD 300% (manufacture of De Sida company, DISPERSE DYES) 3.3owf%, other prescription and method are with embodiment 1.The L value A obtaining is 19, and color fastness to light is more than 4 grades, and washing fastness is 4 grades.Dyefastness is good, compares example 2, and (A-B)=2 meet formula (3): the requirement of-8 < (A-B) < 10, the present invention dyes at normal temperatures and pressures and has splendid color emissivity.
[comparative example 2]
The A silk of selecting does not add 2-methyl isophthalic acid, ammediol, and all the other conditions are with embodiment 2, the polyester composit false twisting silk obtaining.Dyeing temperature is 130 ℃, and L value B is 17, and color fastness to light is 4 grades, and washing fastness is 4 grades.
Be 95 ℃ at dyeing temperature, L value is 20, and color fastness to light is 4 grades, and washing fastness is 3 grades.
[embodiment 3]
Select the copolyester section described in same embodiment 1, then melt spinning under the spinning temperature of 280 ℃, under the high speed traction of 4500m/min, batch, one-step method processing obtains the extension silk of 110dtex/24f, and (its fiber number is 110dtex, fracture strength is 3.8cN/dtex, elongation at break is 36%), this extension silk carries out false twisting processing, the drawing-off multiplying power of false twisting processing is 1.05, rear interlacing pneumatics is 0.2MPa, process velocity is 500m/min, the first hot case employing temperature is the contactless hot case of 390 ℃, obtaining fiber number is 105dtex, fracture strength is 2.8cN/dtex, elongation at break is 21% false twist yarn.The false twist yarn obtaining is carried out to cylinder by method described in embodiment 1 and compile, concise, sizing, dyeing, the processing such as reduction cleaning, dyestuff is Dianix BlackETD 300% (manufacture of De Sida company, DISPERSE DYES) 3.3owf%, other prescription and method are with embodiment 1.The L value A that under 95 ℃ of conditions, dyeing obtains is 20, and color fastness to light is more than 4 grades, and washing fastness is 4 grades.Compare example 3, (A-B)=-5, meet and meet formula (3): the requirement of-8 < (A-B) < 10, the dyeing effect property of the present invention's polyester false twist yarn that dyeability is better than common non-modified at normal temperatures and pressures in the time of high-temp dyeing.
[comparative example 3]
That selects does not add 2-methyl isophthalic acid, ammediol, and all the other conditions are with embodiment 3, the polyester false twist yarn obtaining.L value B when dyeing temperature is 130 ℃ is 25, and color fastness to light is 4 grades, and washing fastness is 3 grades.

Claims (6)

1. a copolyester false-twist yarn, it is characterized in that: in this false twist yarn, at least one is for containing 2-methyl isophthalic acid, the copolyester fiber of ammediol structure, should be containing 2-methyl isophthalic acid, and the percentage by weight that the copolyester fiber of ammediol structure accounts for whole copolyester false-twist yarn is 20~100%; The content that forms the terminal carboxyl group COOH of the polyester of this copolyester false-twist yarn is below 25 equivalents/ton, and in polyester, the content of diethylene glycol (DEG) is below 2.0wt%, and in polyester, the content P of phosphorus atoms and the content M of metallic atom meet formula (1) and formula (2):
5ppm≤[ P ]≤100ppm formula (1)
0.1≤[ M ]/[ P ]≤30 formulas (2).
2. copolyester false-twist yarn according to claim 1, it is characterized in that: this false twist yarn is by the described 2-methyl isophthalic acid that contains, when the copolyester fiber of ammediol structure and other fiber composite, other fiber is nylon fiber, cellulose fibre or cationic fiber, and the percentage by weight that other fibers account for whole copolyester false-twist yarn is 0~80%, does not wherein comprise 0%.
3. copolyester false-twist yarn according to claim 1, is characterized in that: the filament number of this false twist yarn is 0.01~10dtex, and fracture strength is 1.5~5cN/dtex, and elongation at break is 15~40%.
4. copolyester false-twist yarn according to claim 1, it is characterized in that: this false twist yarn adopts the L value A after DISPERSE DYES dyes under the condition of the normal temperature and pressure of 90~100 ℃, L value B after the normal polyester fiber suitable with single fiber quantity with fiber number dyes under 130 ℃ of conditions compares, and meets formula (3):
-8 < (A-B) < 10 formulas (3).
5. a production method for copolyester false-twist yarn claimed in claim 1, is characterized in that:
(1) select the methyl isophthalic acid containing 2-, the polyester slice of ammediol structure, makes copolyesters pre-oriented yarn or extends silk;
(2) the copolyesters pre-oriented yarn of step (1) gained or extension silk are directly carried out to drafting false twisting processing; Or carry out composite drafting false twisting processing with other fibers, obtain product; Wherein drafting false twisting processing conditions is as follows: drawing-off multiplying power is that the 1.0~1.8, first hot case can adopt contact or contactless, and while adopting the hot case of contact, temperature range is 140~250 ℃, and while adopting contactless hot case, temperature range is 280~600 ℃.
6. the production method of copolyester false-twist yarn according to claim 5, it is characterized in that: in described drafting false twisting processing, while using the second hot case, adopt contact or contactless hot case, while selecting the hot case of contact, Temperature Setting scope is 100~230 ℃, 280~600 ℃ of Temperature Setting scopes while adopting contactless hot case.
CN200910174448.4A 2009-11-03 2009-11-03 Copolyester false-twist yarn and production method thereof Expired - Fee Related CN102051706B (en)

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Publication number Priority date Publication date Assignee Title
CN103668555B (en) * 2012-09-12 2017-05-10 东丽纤维研究所(中国)有限公司 Sea-island composite fiber and ultrafine fiber fabric
WO2021097669A1 (en) * 2019-11-19 2021-05-27 江苏盛恒化纤有限公司 Machining process of permanent resilient-type false twist filament
CN114182372A (en) * 2021-10-18 2022-03-15 浙江理工大学 Preparation method of superfine flat yarn

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101063236A (en) * 2007-05-11 2007-10-31 东华大学 Modified copolyester slicer or fabric and method for making same
CN101323996A (en) * 2007-06-14 2008-12-17 东丽纤维研究所(中国)有限公司 Melting processed false twisting yarn, processing method and use
CN101357981A (en) * 2008-08-26 2009-02-04 东华大学 Copolyester section or fiber and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101063236A (en) * 2007-05-11 2007-10-31 东华大学 Modified copolyester slicer or fabric and method for making same
CN101323996A (en) * 2007-06-14 2008-12-17 东丽纤维研究所(中国)有限公司 Melting processed false twisting yarn, processing method and use
CN101357981A (en) * 2008-08-26 2009-02-04 东华大学 Copolyester section or fiber and preparation method thereof

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