CN105177754A - Preparation method of high-tenacity flame-retardant polyester filament - Google Patents
Preparation method of high-tenacity flame-retardant polyester filament Download PDFInfo
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- CN105177754A CN105177754A CN201510688938.1A CN201510688938A CN105177754A CN 105177754 A CN105177754 A CN 105177754A CN 201510688938 A CN201510688938 A CN 201510688938A CN 105177754 A CN105177754 A CN 105177754A
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Abstract
The invention relates to a preparation method of a high-tenacity flame-retardant polyester filament, which comprises the following steps: adding PTA and EG into a charging opening at the front part of a double-screw device for copolymerization to obtain PET; adding a flame retardant and an anti-static agent into a charging opening at the middle part of the double-screw device, blending with PET, and shearing at high temperature to obtain spinning melt; extruding the spinning melt into a spinning component, circularly blowing in the constant temperature and humidity environment, and cooling to obtain nascent fiber; and carrying out first-grade drafting on the nascent fiber through hot oil at 180-200 DEG C, carrying out second-grade drafting on the nascent fiber through boiling water, thermoforming, washing, drying and winding to obtain the high-tenacity flame-retardant polyester filament. The polyester filament obtained by the preparation method provided by the invention has the tenacity of 9-12CN/dtex and the fiber oxygen index of more than 35.9 and is applied to underground coal mines. The device used by the preparation method provided by the invention is simple, convenient in operation and low in price, and the preparation method provides guarantee for technical revolution of the polyester industry.
Description
Technical field
The invention belongs to the preparation method field of terylene thread, particularly a kind of preparation method of high-strength fire-retarding polyester filament.
Background technology
Polyster fibre is fiber with fastest developing speed in various synthetic fiber, output is the highest, consumption is maximum, is the first kind of current synthetic fiber.Its function admirable, cheap, in national defence, industrial cloth and civilian clothes etc., played very large use.Particularly in fiber art, polyester slice obtained by polycondensation makes polyster fibre by melt spinning, this fiber has higher fracture strength and elastic modelling quantity, resilience is moderate, the good characteristic such as fast light, heat-resisting, corrosion-resistant, therefore develops fast from just having obtained since polyster fibre comes out.
Polyster fibre belongs to fusion combustible fibre, and its limited oxygen index only has about 22%, can not meet the requirement of some fields to fire resistance, carries out fire-retardant research seem particularly important to it.Fiber fire-retardant makes the combustibility of fabric in flame reduce, and the rate of fire travel slows down, after flame is removed, fabric can very fast can not resume combustion from put out, prevent the situation of fire or crisis people life security to occur.
Lack hydrophilic radical in terylene molecule, terylene hygroscopicity is very poor, easy balling-up, produces electrostatic.In relative humidity 65%, in the environment that temperature is 25 DEG C, specific volume resistance is up to 10^16 Ω * cm.The occasions such as picture colliery this low humidity, dust are many, easier Accumulating charge, the potential safety hazard such as explosion caused.As compared to the natural fabric such as cotton, fiber crops and real silk, the electrostatic problem of terylene has a strong impact on its industrial development.Therefore, eliminate the electrostatic of terylene, and give its fire resistance, become urgent problem.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of high-strength fire-retarding polyester filament, the polyester filament intensity that the method prepares is up to 9-12CN/dtex, fiber oxygen index (OI) reaches more than 35.9, meet the instructions for use of modernization industry to polyester filament, be applied to underground coal mine.
The preparation method of a kind of high-strength fire-retarding polyester filament of the present invention, comprising:
(1) terephthalic acid (TPA) PTA and ethylene glycol EG is put into the anterior charge door copolymerization of twin screw device, obtain PET; Wherein, the mol ratio of EG and PTA is 1.1 ~ 1.2:1;
(2) charge door in the middle part of twin screw device, adds fire retardant and antistatic additive, blended with PET, and shear at high temperature, obtains spinning melt; Wherein, in twin-screw, temperature is 280-310 DEG C, and pressure is 20-30MPa; The consumption of fire retardant is the 2-8wt% of PTA and EG total amount, and the consumption of antistatic additive is the 1-3wt% of PTA and EG total amount;
(3) clamp-on in filament spinning component by the spinning melt obtained in step (2), ring blowing in the environment of constant temperature and humidity, cooling, obtains as-spun fibre; Wherein, the temperature of ring blowing is 20-30 DEG C, and wind speed is 1-3m/s, and godet roller speed is 800-1500m/min;
(4) by the as-spun fibre in step (3) through the deep fat one-level drawing-off of 180-200 DEG C and the drawing-off of boiling water secondary, HEAT SETTING, washing, dry, winding, obtains high-strength fire-retarding polyester filament.
In described step (1), copolymerization is direct esterification, and reaction temperature is 225-250 DEG C, and pressure is 4-5kg/cm
2, adopt the hot N of continous mode
2protection Code.
In described step (2), fire retardant is polyphosphoric acid amine, antimony pentoxide or polyvinyl chloride.
In described step (2), antistatic additive is polyaniline, shitosan or PMAm.
Described step (1) and the middle twin-screw draw ratio of step (2) are 42 ~ 64, and screw speed is 100 ~ 200rpm.
In described step (3), the environment temperature of constant temperature and humidity is 23 ± 2 DEG C, and humidity is 60 ± 3%.
In described step (3), the spinnerets specification of filament spinning component is 500-3000 hole, and aperture is 0.1-0.4mm.
In described step (4), the drawing roller speed of deep fat one-level drawing-off is 2000-4000m/min, and the drawing roller speed of boiling water secondary drawing-off is 3000-6000m/min, and the draw ratio after secondary drawing-off is 6-10 times.
In described step (4), HEAT SETTING is the hot-air sizing of 80-100 DEG C.
In described step (4), high-strength fire-retarding polyester filament is applied to the clothing fabric of coal miner, the reinforcing material of the helmet, coal mine conveying belt etc.
beneficial effect
(1) preparation method of the present invention have employed syllogic post treatment method and carries out hot-stretch to fiber, and the intensity of fiber is greatly improved, and the polyester filament intensity obtained is up to 9-12CN/dtex, and fiber oxygen index (OI) reaches more than 35.9; Be applied to underground coal mine;
(2) equipment of preparation method's use of the present invention is simple, easy to operate, cheap, for terylene industrial technological revolution provides guarantee;
(3) terylene that preparation method of the present invention obtains is used as the clothing fabric of coal miner, and the reinforcing material of the helmet, coal mine conveying belt etc., wear-resisting solid, flame-retardant and anti-static, the life security for mine workman provides guarantee, has the meaning of particular importance.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
By EG and PTA in molar ratio 1.1:1 add from twin-screw front portion, control condensation temperature 225 DEG C, in screw rod, pressure is 4kg/cm
2, screw slenderness ratio is 42, adopts the hot N of continous mode
2protection.Add the mixture of polyphosphoric acid amine-polyaniline from the middle part of twin-screw, the consumption of polyphosphoric acid amine is the 2wt% of PTA and EG total amount, and the consumption of polyaniline is the 1wt% of PTA and EG total amount.In twin-screw, temperature is 280 DEG C, and pressure is 20MPa, and screw speed is 100r/min.
The molten state spinning solution obtained is clamp-oned in filament spinning component, and spinnerets specification is 500 holes, and aperture is 0.4mm, and the temperature of spinning chamber is 23 ± 2 DEG C, and humidity is 60 ± 3%.Spinning ring blowing temperature is 20 DEG C, and wind speed is 1m/s.Godet roller speed is 800m/min.As-spun fibre is carried out one-level drawing-off in the deep fat of 180 DEG C, and drawing roller speed is 2000m/min; Again polyster fibre is carried out secondary drawing-off in boiling water, drawing roller speed is 3000m/min, and total stretch ratio is 6 times.Again after the hot-air sizing of 80 DEG C, washing, dry, reel stand-by.Obtain the high-strength fire-retarding polyester filament that intensity is 9CN/dtex, limited oxygen index is 35.9%.
Embodiment 2
By EG and PTA in molar ratio 1.1:1 add from twin-screw front portion, control condensation temperature 230 DEG C, in screw rod, pressure is 4kg/cm
2, screw slenderness ratio is 50, adopts the hot N of continous mode
2protection.Add the mixture of polyphosphoric acid amine-polyaniline from the middle part of twin-screw, the consumption of polyphosphoric acid amine is the 7wt% of PTA and EG total amount, and the consumption of polyaniline is the 1wt% of PTA and EG total amount.In twin-screw, temperature is 280 DEG C, and pressure is 20MPa, and screw speed is 120r/min.
The molten state spinning solution obtained is clamp-oned in filament spinning component, and spinnerets specification is 1000 holes, and aperture is 0.4mm, and the temperature of spinning chamber is 23 ± 2 DEG C, and humidity is 60 ± 3%.Spinning ring blowing temperature is 20 DEG C, and wind speed is 1m/s.Godet roller speed is 1000m/min.As-spun fibre is carried out one-level drawing-off in the deep fat of 180 DEG C, and drawing roller speed is 3000m/min; Again polyster fibre is carried out secondary drawing-off in boiling water, drawing roller speed is 3000m/min, and total stretch ratio is 6.5 times.Again after the hot-air sizing of 80 DEG C, washing, dry, reel stand-by.Obtain the high-strength fire-retarding polyester filament that intensity is 9CN/dtex, limited oxygen index is 39.4%.
Embodiment 3
By EG and PTA in molar ratio 1.15:1 add from twin-screw front portion, control condensation temperature 240 DEG C, in screw rod, pressure is 4.5kg/cm
2, screw slenderness ratio is the hot N of 55 employing continous mode
2protection.Add the mixture of antimony pentoxide-shitosan from the middle part of twin-screw, the consumption of antimony pentoxide is the 4wt% of PTA and EG total amount, and the consumption of polyaniline is the 2wt% of PTA and EG total amount.In twin-screw, temperature is 285 DEG C, and pressure is 25MPa, and screw speed is 140r/min.
The molten state spinning solution obtained is clamp-oned in filament spinning component, and spinnerets specification is 1500 holes, and aperture is 0.3mm, and the temperature of spinning chamber is 23 ± 2 DEG C, and humidity is 60 ± 3%.Spinning ring blowing temperature is 25 DEG C, and wind speed is 2m/s.Godet roller speed is 1200m/min.As-spun fibre is carried out one-level drawing-off in the deep fat of 190 DEG C, and drawing roller speed is 4000m/min; Again polyster fibre is carried out secondary drawing-off in boiling water, drawing roller speed is 4000m/min, and total stretch ratio is 7 times.Again after the hot-air sizing of 90 DEG C, washing, dry, reel stand-by.Obtain the high-strength fire-retarding polyester filament that intensity is 9.5CN/dtex, limited oxygen index is 36.5%.
Embodiment 4
By EG and PTA in molar ratio 1.15:1 add from twin-screw front portion, control condensation temperature 245 DEG C, in screw rod, pressure is 4.5kg/cm
2, screw slenderness ratio is the hot N of 58 employing continous mode
2protection.Add the mixture of antimony pentoxide-shitosan from the middle part of twin-screw, the consumption of antimony pentoxide is the 4.5wt% of PTA and EG total amount, and the consumption of polyaniline is the 3wt% of PTA and EG total amount.In twin-screw, temperature is 290 DEG C, and pressure is 25MPa, and screw speed is 150r/min.
The molten state spinning solution obtained is clamp-oned in filament spinning component, and spinnerets specification is 2000 holes, and aperture is 0.2mm, and the temperature of spinning chamber is 23 ± 2 DEG C, and humidity is 60 ± 3%.Spinning ring blowing temperature is 25 DEG C, and wind speed is 2m/s.Godet roller speed is 1400m/min.As-spun fibre is carried out one-level drawing-off in the deep fat of 190 DEG C, and drawing roller speed is 4500m/min; Again polyster fibre is carried out secondary drawing-off in boiling water, drawing roller speed is 4000m/min, and total stretch ratio is 8 times.Again after the hot-air sizing of 90 DEG C, washing, dry, reel stand-by.Obtain high-strength fire-retarding polyester filament that intensity is 10CN/dtex, limited oxygen index is 37.2%.
Embodiment 5
By EG and PTA in molar ratio 1.2:1 add from twin-screw front portion, control condensation temperature 250 DEG C, in screw rod, pressure is 5kg/cm
2, screw slenderness ratio is the hot N of 60 employing continous mode
2protection.Add the mixture of polyvinyl chloride-PMAm from the middle part of twin-screw, the consumption of polyvinyl chloride is the 6wt% of PTA and EG total amount, and the consumption of PMAm is the 1wt% of PTA and EG total amount.In twin-screw, temperature is 300 DEG C, and pressure is 30MPa, and screw speed is 200r/min.
The molten state spinning solution obtained is clamp-oned in filament spinning component, and spinnerets specification is 2500 holes, and aperture is 0.1mm, and the temperature of spinning chamber is 23 ± 2 DEG C, and humidity is 60 ± 3%.Spinning ring blowing temperature is 30 DEG C, and wind speed is 3m/s.Godet roller speed is 1500m/min.As-spun fibre is carried out one-level drawing-off in the deep fat of 190 DEG C, and drawing roller speed is 5000m/min; Again polyster fibre is carried out secondary drawing-off in boiling water, drawing roller speed is 5000m/min, and total stretch ratio is 9 times.Again after the hot-air sizing of 100 DEG C, washing, dry, reel stand-by.Obtain the high-strength fire-retarding polyester filament that intensity is 11CN/dtex, limited oxygen index is 38.6%.
Embodiment 6
By EG and PTA in molar ratio 1.2:1 add from twin-screw front portion, control condensation temperature 250 DEG C, in screw rod, pressure is 5kg/cm
2, screw slenderness ratio is the hot N of 64 employing continous mode
2protection.Add the mixture of polyvinyl chloride-PMAm from the middle part of twin-screw, the consumption of polyvinyl chloride is the 8wt% of PTA and EG total amount, and the consumption of PMAm is the 1wt% of PTA and EG total amount.In twin-screw, temperature is 310 DEG C, and pressure is 30MPa, and screw speed is 200r/min.
The molten state spinning solution obtained is clamp-oned in filament spinning component, and spinnerets specification is 3000 holes, and aperture is 0.1mm, and the temperature of spinning chamber is 23 ± 2 DEG C, and humidity is 60 ± 3%.Spinning ring blowing temperature is 30 DEG C, and wind speed is 3m/s.Godet roller speed is 1500m/min.As-spun fibre is carried out one-level drawing-off in the deep fat of 190 DEG C, and drawing roller speed is 5000m/min; Again polyster fibre is carried out secondary drawing-off in boiling water, drawing roller speed is 6000m/min, and total stretch ratio is 10 times.Again after the hot-air sizing of 100 DEG C, washing, dry, reel stand-by.Obtain the high-strength fire-retarding polyester filament that intensity is 12CN/dtex, limited oxygen index is 39.1%.
Claims (10)
1. a preparation method for high-strength fire-retarding polyester filament, comprising:
(1) terephthalic acid (TPA) PTA and ethylene glycol EG is put into the anterior charge door copolymerization of twin screw device, obtain PET; Wherein, the mol ratio of EG and PTA is 1.1 ~ 1.2:1;
(2) charge door in the middle part of twin screw device, adds fire retardant and antistatic additive, blended with PET, and shear at high temperature, obtains spinning melt; Wherein, in twin-screw, temperature is 280-310 DEG C, and pressure is 20-30MPa; The consumption of fire retardant is the 2-8wt% of PTA and EG total amount, and the consumption of antistatic additive is the 1-3wt% of PTA and EG total amount;
(3) clamp-on in filament spinning component by the spinning melt obtained in step (2), ring blowing in the environment of constant temperature and humidity, cooling, obtains as-spun fibre; Wherein, the temperature of ring blowing is 20-30 DEG C, and wind speed is 1-3m/s, and godet roller speed is 800-1500m/min;
(4) by the as-spun fibre in step (3) through the deep fat one-level drawing-off of 180-200 DEG C and the drawing-off of boiling water secondary, HEAT SETTING, washing, dry, winding, obtains high-strength fire-retarding polyester filament.
2. the preparation method of a kind of high-strength fire-retarding polyester filament according to claim 1, is characterized in that, in described step (1), copolymerization is direct esterification, and reaction temperature is 225-250 DEG C, and pressure is 4-5kg/cm
2, adopt the hot N of continous mode
2protection Code.
3. the preparation method of a kind of high-strength fire-retarding polyester filament according to claim 1, is characterized in that, in described step (2), fire retardant is polyphosphoric acid amine, antimony pentoxide or polyvinyl chloride.
4. the preparation method of a kind of high-strength fire-retarding polyester filament according to claim 1, is characterized in that, in described step (2), antistatic additive is polyaniline, shitosan or PMAm.
5. the preparation method of a kind of high-strength fire-retarding polyester filament according to claim 1, is characterized in that, described step (1) and the middle twin-screw draw ratio of step (2) are 42 ~ 64, and screw speed is 100 ~ 200rpm.
6. the preparation method of a kind of high-strength fire-retarding polyester filament according to claim 1, is characterized in that, in described step (3), the environment temperature of constant temperature and humidity is 23 ± 2 DEG C, and humidity is 60 ± 3%.
7. the preparation method of a kind of high-strength fire-retarding polyester filament according to claim 1, is characterized in that, in described step (3), the spinnerets specification of filament spinning component is 500-3000 hole, and aperture is 0.1-0.4mm.
8. the preparation method of a kind of high-strength fire-retarding polyester filament according to claim 1, it is characterized in that, in described step (4), the drawing roller speed of deep fat one-level drawing-off is 2000-4000m/min, the drawing roller speed of boiling water secondary drawing-off is 3000-6000m/min, and the draw ratio after secondary drawing-off is 6-10 times.
9. the preparation method of a kind of high-strength fire-retarding polyester filament according to claim 1, is characterized in that, in described step (4), HEAT SETTING is the hot-air sizing of 80-100 DEG C.
10. the preparation method of a kind of high-strength fire-retarding polyester filament according to claim 1, is characterized in that, in described step (4), high-strength fire-retarding polyester filament is applied to the clothing fabric of coal miner, the reinforcing material of the helmet or coal mine conveying belt.
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Cited By (9)
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| CN105780260A (en) * | 2016-04-29 | 2016-07-20 | 王斐芬 | Flame-retardant polysulfonamide blended fabric |
| CN107190358A (en) * | 2017-06-30 | 2017-09-22 | 太仓红桥服饰有限公司 | A kind of environment-friendly antibacterial anti-radiation garment fabric |
| CN107201568A (en) * | 2017-06-30 | 2017-09-26 | 太仓红桥服饰有限公司 | A kind of environment-friendly antibacterial Anti-ultraviolet Garment Fabric |
| CN107268114A (en) * | 2017-06-30 | 2017-10-20 | 太仓红桥服饰有限公司 | A kind of environment-friendly antibacterial deodorization garment material |
| CN108699730A (en) * | 2016-02-29 | 2018-10-23 | 阿克萨丙烯酸化工股份有限公司 | The fiber made of ter-polymers mixture |
| CN109505025A (en) * | 2018-11-27 | 2019-03-22 | 华叶莹 | A kind of anti-fire modified PET fiber and preparation method thereof |
| CN109736083A (en) * | 2018-12-29 | 2019-05-10 | 中润科技股份有限公司 | A kind of nano modification bidirectional inductive Far Infrared Polyester Fiber long filament and its preparation process |
| CN111607968A (en) * | 2020-05-29 | 2020-09-01 | 江苏万邦特种纺织发展有限公司 | Manufacturing process of anti-wicking polyester filament |
| CN112962159A (en) * | 2021-03-01 | 2021-06-15 | 太仓逸枫化纤有限公司 | High-strength polyester filament yarn, preparation method and preparation device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108699730A (en) * | 2016-02-29 | 2018-10-23 | 阿克萨丙烯酸化工股份有限公司 | The fiber made of ter-polymers mixture |
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| CN107268114A (en) * | 2017-06-30 | 2017-10-20 | 太仓红桥服饰有限公司 | A kind of environment-friendly antibacterial deodorization garment material |
| CN109505025A (en) * | 2018-11-27 | 2019-03-22 | 华叶莹 | A kind of anti-fire modified PET fiber and preparation method thereof |
| CN109736083A (en) * | 2018-12-29 | 2019-05-10 | 中润科技股份有限公司 | A kind of nano modification bidirectional inductive Far Infrared Polyester Fiber long filament and its preparation process |
| CN111607968A (en) * | 2020-05-29 | 2020-09-01 | 江苏万邦特种纺织发展有限公司 | Manufacturing process of anti-wicking polyester filament |
| CN112962159A (en) * | 2021-03-01 | 2021-06-15 | 太仓逸枫化纤有限公司 | High-strength polyester filament yarn, preparation method and preparation device |
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