CN1362548A - Cationic dye for copolyester slice and fiber and its prepn. - Google Patents
Cationic dye for copolyester slice and fiber and its prepn. Download PDFInfo
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- CN1362548A CN1362548A CN 02110770 CN02110770A CN1362548A CN 1362548 A CN1362548 A CN 1362548A CN 02110770 CN02110770 CN 02110770 CN 02110770 A CN02110770 A CN 02110770A CN 1362548 A CN1362548 A CN 1362548A
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Abstract
The present invention relates to a kind of cation-dyeable copolyester chip of fibre produced by copolymerization of terephthalic acid monomer, ethylene ester isophthalate-5-sodium sulfonate (potassium sulfonate) monomer and glycol monomer and its preparation method. Said ivnention fibre features cation-dyeability of normal temp. and normal pressure, high contractility, soft hand touch and resisting fuzzy and pilling, can be extensively used for pure yarn or blending with natural fibres of silk, cotton, wool and bast fibre to obtain various shell fabrics.
Description
Technical field
The present invention relates to a kind of synthetic fiber, specifically a kind of copolyester section of cation dye chromophil or fiber and preparation method.
Background technology
Terylene is be raw material with the polyester through melt spinning and after the prepared fiber of processing.It is synthetic and be spun into fiber with aliphatic diacid and aliphatic diol by the Tomas Carothers of E.I.Du Pont Company that polyester the earliest is nineteen twenty-eight.But this polyester fiber fusing point low (～65 ℃), facile hydrolysis, not alkaline-resisting, no practical value.Nineteen forty-one, the persons such as Wen Feierde of Britain synthesized Polyethyleneglycol Terephthalate with aromatic terephthalic acid (TPA) (PTA) and ethylene glycol (EG), and successfully made the fiber with practical value, and its fusing point is higher than 250 ℃, is named as terylene (Terylene).Nineteen fifty-one, du pont company was trade name with Da Kelun (Dacron), and built up the polyester fiber factory of the first in the world man that produces 1.6 ten thousand tons per year in nineteen fifty-three.The physical and mechanical properties excellence of terylene, the elastic modelling quantity height, heat resistance is good, and is quick-drying washable; The plasticity of physical and mechanical properties is big, utilize different processing technologys can produce can with natural fibre blended staple fibres such as cotton, hair, fiber crops, also can produce long filament for woven or knitting.Therefore, polyester fiber has worldwide obtained development rapidly.
Although the physical and mechanical property of polyester fiber and comprehensive wearing characteristics are good, but because the tight packing of polyester molecule chain, the degree of crystallinity and the degree of orientation are higher, polarity is less, lacks hydrophily, the gap that does not have suitably to hold dye molecule between the tortuous long-chain molecule of polyester, therefore dye particles is difficult for penetrating fiber, its dyeability is poor, can use the kind of dyestuff few, and polyester fiber can only adopt methods such as DISPERSE DYES carrier dyeing, high-temp dyeing and pad-dry-cure dyeing.
Summary of the invention
The copolyester section or the fiber that the purpose of this invention is to provide a kind of cation dye chromophil.
Another object of the present invention provides a kind of copolyester section or fiber production method of above-mentioned cation dye chromophil
The copolyester section of cation dye chromophil of the present invention or fiber, it is the copolymer of terephthalic acid (TPA), ethylene glycol, ethylene m-phthalate-5-sodium sulfonate or potassium, the monomer mole ratio of terephthalic acid monomers, ethylene glycol is 1 in the polymer: 1.7-2.4, the monomer of ethylene m-phthalate-5-sodium sulfonate or potassium is 2.4%～18% molar weight of terephthalic acid monomers.
The copolyester section of above-mentioned cation dye chromophil of the present invention or fiber production method are to be made by following method respectively:
Divalence, trivalent, tetravalent metal etc. in the presence of oxide and the acetate catalyst thereof and 220～260 ℃, terephthalic acid (TPA) and ethylene glycol monomer mol ratio are 1: reaction 1～5 hour and dehydration during 1.7-2.4, adding ethylene m-phthalate-5-sodium sulfonate or potassium, at 250-300 ℃ of copolymer-1-4 hour, make the copolyester section of cation dye chromophil, wherein catalyst amount is the 0.01%-0.08% of terephthalic acid (TPA) weight, and the monomer of ethylene m-phthalate-5-sodium sulfonate or potassium is 2.4%～18% molar weight of terephthalic acid monomers.Described divalence, trivalent, tetravalent metal can be Na
+, Ga
2+, Mn
4+, Co
2+, Zn
2+
The copolyester section of above-mentioned cation dye chromophil is obtained dried section 130-180 ℃ of drying,
Above-mentioned section or dried section are carried out the copolyester fiber that spinning obtains cation dye chromophil in following condition: 280～320 ℃ of extruder temperatures, spinning speed 900-5000m/min, draft temperature 65-180 ℃, draw ratio is 1.5-5 times.
Owing to introduced sodium group, the metal ion (Na on it in this condensate
+, K
+Deng) easily and the cation exchange in the cation dyes, dyestuff just is fixed on the polyester molecule with ionic bond, disengage salt simultaneously, because dyeing is carried out in water-bath, NaCl etc. can remove fully, balance is carried out to helping the direction that dyestuff is combined on the fiber always, and the dyeability of polyester fiber is improved.
Fiber provided by the present invention can dye with the cation dyes normal temperature and pressure.And because SiPM has destroyed the macromolecular regularity of PET condensate, make the condensate crystalline rate slack-off, copolymer institute spinning fibre is soft, gloss is soft, simultaneously can give fiber highly shrinkable and anti-fluffing and anti-pilling performance by the optimizing and revising of spinning technique.
The copolyester fiber of cation dye chromophil of the present invention is the serial fiber of a kind of multifunctionality, can be the staple fibre of cation dyes normal-temperature normal-pressure dyeable, the anti-fluffing and anti-pilling staple fibre of cation dyes normal-temperature normal-pressure dyeable or the high shrinkage short fiber of cation dyes normal-temperature normal-pressure dyeable; The low speed that is a kind of cation dyes normal-temperature normal-pressure dyeable spins drawing of fiber; Be that a kind of high-speed spinning drawing of fiber of cation dyes normal-temperature normal-pressure dyeable, the high-speed spinning of cation dyes normal-temperature normal-pressure dyeable add the height contraction long fiber of the full drawing of fiber of high-speed spinning of elastic fibre or cation dyes normal-temperature normal-pressure dyeable, a kind of cation dyes normal-temperature normal-pressure dyeable or the anti-fluffing and anti-pilling long fiber of cation dyes normal-temperature normal-pressure dyeable; The thin dawn multifilament or the monofilament of cation dyes normal-temperature normal-pressure dyeable; The special-shaped cation dyes normal-temperature normal-pressure dyeable fiber of cation dyes normal-temperature normal-pressure dyeable.And section of the present invention can with polyester, the polyamide blended functional fiber that is spun into.
The fiber of invention has the cation dyes normal-temperature normal-pressure dyeable, highly shrinkable, fabrics feel soft, characteristics such as anti-fluffing and anti-pilling, and has an environmental safety, can produce in enormous quantities effectively, can be widely used in pure spin or natural fibre blended, to obtain the wearing fabric of style varied with silk, thin,tough silk, cotton, hair, fiber crops etc.
Most preferred embodiment
Further specify the present invention with the following example, but the present invention is not limited to these embodiment.
Embodiment 1
Adopt batch (-type) polyester equipment, PTA, EG add catalyst S bAc simultaneously in adding
3400g stirs 3h down at 240-250 ℃, treat that water yield reaches 90% o'clock of theoretical value, interpolation contains the SiPM ethylene glycol solution that is equivalent to the PTA2.4 molar percentage and carries out polycondensation reaction, temperature is controlled at 270-300 ℃, vacuum＜1mmHg, can make the copolymer inherent viscosity is 0.62, Tm=250 ℃.
Embodiment 2
Adopt batch (-type) polyester equipment, after PTA, EG esterification are finished, add and contain the SiPM ethylene glycol solution that is equivalent to the PTA3.6 molar percentage, through fully stirring polycondensation, Tm=248 ℃ of discharging copolyester section, [η]=0.60.
Embodiment 3
Adopt batch (-type) polyester equipment, after PTA, EG esterification are finished, add and contain the SiPM ethylene glycol solution that is equivalent to the PTA7.2 molar percentage, through fully stirring polycondensation, Tm=238 ℃ of discharging copolyester section, [η]=0.54.
Embodiment 4
Adopt batch (-type) polyester equipment, after PTA, EG esterification are finished, add and contain the SiPM ethylene glycol solution that is equivalent to the PTA10.8 molar percentage, through fully stirring polycondensation, Tm=230 ℃ of discharging copolyester section, [η]=0.50.
Embodiment 5
Adopt batch (-type) polyester equipment, after PTA, EG esterification are finished, add and contain the SiPM ethylene glycol solution that is equivalent to the PTA14.4 molar percentage, through fully stirring polycondensation, Tm=223 ℃ of discharging copolyester section, [η]=0.45.
Embodiment 6
Adopt batch (-type) polyester equipment, after PTA, EG esterification are finished, add and contain the SiPM ethylene glycol solution that is equivalent to the PTA18 molar percentage, through fully stirring polycondensation, Tm=218 ℃ of discharging copolyester section, [η]=0.38.
Embodiment 7
With copolyester section in the vacuum drum drier, steam pressure 0.2Mpa, vacuum≤-0.097Mpa, slowly heat up, control pre-crystallizing and drying 16～20hr cool time, obtain the dried section of moisture content less than 50PPM.
Embodiment 8
Adopt VD406 spinning combination machine and LVD801 after-processing combination machine, 290～320 ℃ of control extruder temperatures, winding speed 1000m/min, 25～30 ℃ of cooling wind-warm syndrome, 3.8～4.2 times of draw ratios, stretching distribution ratio 70～80%, 70 ℃ of stretch bath temperature, 90～130 ℃ of relaxation heat setting temperature, relaxation heat setting time 30～40min, obtain fibrous fracture intensity 3.8CN/dt, elongation at break is the staple fibre of 24.8% cation dyes normal-temperature normal-pressure dyeable.
Embodiment 9
Adopt VD406 spinning combination machine and LVD801 after-processing combination machine, 290～320 ℃ of control extruder temperatures, winding speed 1000m/min, 25～30 ℃ of cooling wind-warm syndrome, 3.8～4.2 times of draw ratios, stretching distribution ratio 70～80%, 70 ℃ of stretch bath temperature, 90～130 ℃ of relaxation heat setting temperature, relaxation heat setting time 30～40min, obtain fibrous fracture intensity 2.8CN/dt, elongation at break is 23.7%, and anti-fluffing and anti-pilling is 4 grades a cation dyes normal-temperature normal-pressure dyeable anti-fluffing and anti-pilling staple fibre.
Embodiment 10
Adopt VD406 spinning combination machine and LVD801 after-processing combination machine, 290～320 ℃ of control extruder temperatures, winding speed 1000m/min, 25～30 ℃ of cooling wind-warm syndrome, 3.8～4.2 times of draw ratios, stretching distribution ratio 70～80%, 60 ℃ of stretch bath temperature, 90～130 ℃ of relaxation heat setting temperature, relaxation heat setting time 30～40min, obtain fibrous fracture intensity 3.8CN/dt, elongation at break is 24.8%, and boiling water shrinkage is 35% cation dyes normal-temperature normal-pressure dyeable high shrinkage short fiber.
Embodiment 11
Adopt VC406 spinning machine and KJKV518 drawing machine, 290～320 ℃ of control extruder temperatures, winding speed 900m/min, draw ratio 2.5～3.5,80～180 ℃ of draft temperatures obtain fibrous fracture intensity 3CN/dt, the drawn yarn of the cation dyes normal-temperature normal-pressure dyeable of extension at break 30.2%.
Embodiment 12
Adopt VC406 spinning machine and KJKV518 drawing machine, 290～320 ℃ of control extruder temperatures, winding speed 900m/min, draw ratio 2.5～3.5,80～180 ℃ of draft temperatures, obtain fibrous fracture intensity 2.5CN/dt, extension at break 28.2%, anti-fluffing and anti-pilling are the drawn yarn of 4 grades cation dyes normal-temperature normal-pressure dyeable.
Embodiment 13
Adopt VC406 spinning machine and KJKV518 drawing machine, 290～320 ℃ of control extruder temperatures, winding speed 900m/min, draw ratio 2.5～3.5,70～160 ℃ of draft temperatures, obtain fibrous fracture intensity 2.5CN/dt, extension at break 28.2%, boiling water shrinkage is the high contraction stretching silk of 30% cation dyes normal-temperature normal-pressure dyeable.
Embodiment 14
Adopt KF spinning machine and Zinser517/2 type drawing machine, 290～320 ℃ of control extruder temperatures, winding speed 3200m/min, draw ratio 1.5～1.8,70～150 ℃ of heat dish, hot plate temperatures, obtain fibrous fracture intensity 3.2CN/dt, extension at break 28.2%, the high-speed spinning drawn yarn of cation dyes normal-temperature normal-pressure dyeable.
Embodiment 15
Adopt KF spinning machine and KF6M-700 elasticizer, 290～320 ℃ of control extruder temperatures, winding speed 3200m/min, draw ratio 1.5～1.8,70～160 ℃ of first, second heater temperatures, obtain fibrous fracture intensity 3.3CN/dt, the high-speed spinning of extension at break 26.4% cation dyes normal-temperature normal-pressure dyeable adds elater.
Embodiment 16
Adopt KF spinning machine and Barmag up-coiler, 290～320 ℃ of control extruder temperatures, winding speed 4200m/min, 70～150 ℃ of first, second draw-off godet temperature, obtain fracture strength 3.3CN/dt, the high-speed spinning fullly drawn yarn (FDY) of extension at break 29.4% cation dyes normal-temperature normal-pressure dyeable.
Embodiment 17
Adopt ABS spinning machine and Barmag drawing machine, 290～320 ℃ of control extruder temperatures, winding speed 1000m/min, 70～140 ℃ of heat dish, hot plate temperatures, obtain fiber number 35dt/12F, fracture strength 3.0CN/dt, extension at break 29.4% cation dyes normal-temperature normal-pressure dyeable fiber.
Embodiment 18
Adopt ABS spinning machine and Barmag drawing machine, 290～320 ℃ of control extruder temperatures, winding speed 1000m/min, 70～140 ℃ of heat dish, hot plate temperatures, obtain fiber number 33dt/1F, fracture strength 2.9CN/dt, extension at break 25.4% cation dyes normal-temperature normal-pressure dyeable fiber.
Claims (8)
1. the copolyester section of a cation dye chromophil or fiber, it is the copolymer of terephthalic acid (TPA), ethylene glycol, ethylene m-phthalate-5-sodium sulfonate or potassium, the monomer mole ratio of terephthalic acid monomers, ethylene glycol is 1 in the polymer: 1.7-2.4, the monomer of ethylene m-phthalate-5-sodium sulfonate or potassium is the 2.4%-18% molar weight of terephthalic acid monomers.
2. the copolyester section of a cation dye chromophil as claimed in claim 1 or fiber is characterized in that described fiber is a kind of staple fibre of cation dyes normal-temperature normal-pressure dyeable, the anti-fluffing and anti-pilling staple fibre of cation dyes normal-temperature normal-pressure dyeable or the high shrinkage short fiber of cation dyes normal-temperature normal-pressure dyeable.
3. the copolyester section of a cation dye chromophil as claimed in claim 1 or fiber is characterized in that described fiber is that a kind of low speed of cation dyes normal-temperature normal-pressure dyeable spins drawing of fiber.
4. the copolyester section of a cation dye chromophil as claimed in claim 1 or fiber is characterized in that described fiber is that a kind of high-speed spinning drawing of fiber of cation dyes normal-temperature normal-pressure dyeable, the high-speed spinning of cation dyes normal-temperature normal-pressure dyeable add the full drawing of fiber of high-speed spinning of elastic fibre or cation dyes normal-temperature normal-pressure dyeable.
5. the copolyester section of a cation dye chromophil as claimed in claim 1 or fiber is characterized in that described fiber is a kind of height contraction long fiber of cation dyes normal-temperature normal-pressure dyeable or the anti-fluffing and anti-pilling long fiber of cation dyes normal-temperature normal-pressure dyeable.
6. the copolyester section of a cation dye chromophil as claimed in claim 1 or fiber is characterized in that described fiber is a kind of thin dawn multifilament or monofilament of cation dyes normal-temperature normal-pressure dyeable.
7. adopt a kind of copolyester section or fiber of cation dye chromophil as claimed in claim 1, it is characterized in that described fiber is a kind of profiled filament of cation dyes normal-temperature normal-pressure dyeable.
8. the copolyester section of a cation dye chromophil as claimed in claim 1 or fiber preparation method is characterized in that described fiber is to be made by following method respectively:
In the presence of two-tetravalent metal oxide and acetate catalyst thereof and 220～260 ℃, terephthalic acid (TPA) and ethylene glycol monomer mol ratio are 1: reaction 1～5 hour and dehydration during 1.7-2.4, adding ethylene m-phthalate-5-sodium sulfonate or potassium, at 250-300 ℃ of copolymer-1-4 hour, make the copolyester section of cation dye chromophil, wherein catalyst amount is the 0.01%-0.08% of terephthalic acid (TPA) weight, and the monomer of ethylene m-phthalate-5-sodium sulfonate or potassium is 2.4%～18% molar weight of terephthalic acid monomers; The copolyester section of above-mentioned cation dye chromophil is obtained dried section 130-180 ℃ of drying;
Above-mentioned section or dried section are carried out the copolyester fiber that spinning obtains cation dye chromophil in following condition: 280～320 ℃ of extruder temperatures, spinning speed 900-5000m/min, draft temperature 65-180 ℃, draw ratio is 1.5-5 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02110770 CN1362548A (en) | 2002-02-05 | 2002-02-05 | Cationic dye for copolyester slice and fiber and its prepn. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02110770 CN1362548A (en) | 2002-02-05 | 2002-02-05 | Cationic dye for copolyester slice and fiber and its prepn. |
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| Publication Number | Publication Date |
|---|---|
| CN1362548A true CN1362548A (en) | 2002-08-07 |
Family
ID=4741238
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02110770 Pending CN1362548A (en) | 2002-02-05 | 2002-02-05 | Cationic dye for copolyester slice and fiber and its prepn. |
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|---|---|
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100345883C (en) * | 2004-05-10 | 2007-10-31 | （株）晓星 | Flame retardant polyesterpolymer able to dye by using cation pigment,its mfg.method and copolymer fiber using the same |
| CN100348641C (en) * | 2004-11-12 | 2007-11-14 | 中国石油天然气集团公司 | Alkali soluble polyester chip and its prepn |
| CN100413907C (en) * | 2004-09-16 | 2008-08-27 | 洛阳高新技术开发区南峰聚酯有限公司 | Cation dye normal pressure deep dyeing estercopolymer and its preparing method |
| CN102080285A (en) * | 2010-12-21 | 2011-06-01 | 浙江恒逸聚合物有限公司 | Production method of spunbonded polyester embroidery thread and product of same |
| CN101492841B (en) * | 2009-03-05 | 2011-07-27 | 绍兴文理学院 | Hollow micropore special-shaped polyester fiber and methods for making same |
| CN102199808A (en) * | 2011-03-29 | 2011-09-28 | 东华大学 | Method for preparing cationic dye deeply dyed copolyester fibers at normal pressure |
| CN102418165B (en) * | 2008-01-08 | 2014-04-09 | 帝人纤维株式会社 | Normal pressure cation dyeable polyester and fiber |
| CN106827709A (en) * | 2017-03-23 | 2017-06-13 | 上海题桥纺织染纱有限公司 | Three-dimensional wrinkle flower skin texture warming knitted composite fabric of embossment of a kind of high convergency and preparation method thereof |
| CN109457351A (en) * | 2018-11-13 | 2019-03-12 | 南通双弘纺织有限公司 | The cation-modified polyester of normal-pressure easy-to-dye and cotton blending yarn |
-
2002
- 2002-02-05 CN CN 02110770 patent/CN1362548A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100345883C (en) * | 2004-05-10 | 2007-10-31 | （株）晓星 | Flame retardant polyesterpolymer able to dye by using cation pigment,its mfg.method and copolymer fiber using the same |
| CN100413907C (en) * | 2004-09-16 | 2008-08-27 | 洛阳高新技术开发区南峰聚酯有限公司 | Cation dye normal pressure deep dyeing estercopolymer and its preparing method |
| CN100348641C (en) * | 2004-11-12 | 2007-11-14 | 中国石油天然气集团公司 | Alkali soluble polyester chip and its prepn |
| CN102418165B (en) * | 2008-01-08 | 2014-04-09 | 帝人纤维株式会社 | Normal pressure cation dyeable polyester and fiber |
| CN101492841B (en) * | 2009-03-05 | 2011-07-27 | 绍兴文理学院 | Hollow micropore special-shaped polyester fiber and methods for making same |
| CN102080285A (en) * | 2010-12-21 | 2011-06-01 | 浙江恒逸聚合物有限公司 | Production method of spunbonded polyester embroidery thread and product of same |
| CN102080285B (en) * | 2010-12-21 | 2012-01-25 | 浙江恒逸聚合物有限公司 | Production method of spunbonded polyester embroidery thread and product of same |
| CN102199808A (en) * | 2011-03-29 | 2011-09-28 | 东华大学 | Method for preparing cationic dye deeply dyed copolyester fibers at normal pressure |
| CN106827709A (en) * | 2017-03-23 | 2017-06-13 | 上海题桥纺织染纱有限公司 | Three-dimensional wrinkle flower skin texture warming knitted composite fabric of embossment of a kind of high convergency and preparation method thereof |
| CN106827709B (en) * | 2017-03-23 | 2019-04-23 | 上海题桥纺织染纱有限公司 | Warming knitted composite fabric of a kind of high convergency solid wrinkle flower skin texture embossment and preparation method thereof |
| CN109457351A (en) * | 2018-11-13 | 2019-03-12 | 南通双弘纺织有限公司 | The cation-modified polyester of normal-pressure easy-to-dye and cotton blending yarn |
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