CN103088454B - Production method of melt direct spinning high-modulus low-shrinkage polyester industrial filament - Google Patents
Production method of melt direct spinning high-modulus low-shrinkage polyester industrial filament Download PDFInfo
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Abstract
The invention discloses a production method of a melt direct spinning high-modulus low-shrinkage polyester industrial filament, and belongs to the technical field of polyester industrial yarns. The production method is used for a tyre cord. The method comprises melt liquid tackifying, melt direct spinning, draft heat shaping and winding molding. A spinning machine is four heads/ position and six heads/position, due to the fact that melt direct spinning is achieved, and limit of the flow of spinning by a spinning screw does not exist. High-modulus low-shrinkage polyester industrial filaments produced according to the technical scheme of the production method are stable in product quality and high in production efficiency, improve the yield of unit time, and lower production energy consumption and production cost. Products can be used as good materials such as tyre cords, geogrids and polyester cords.
Description
Technical field
The present invention relates to fiber product manufacturing technology field, be specifically related to a kind of production method of fused mass directly spinning HMLS Polyester industrial filament.
Background technology
High modulus low shrinkage polyester industrial filament, being called for short High Modulus And Low Shrinkage polyester industrial filament is the industrial filament with higher initial modulus and lower percent thermal shrinkage, its good mechanical properties, there is the structure of high-crystallinity, high-orientation and high regularity and lower inside residual mechanical stress, be mainly used in rubber framework material, as automobile cord fabric and cotton rope etc.The production of current High Modulus And Low Shrinkage polyester industrial fiber mostly is microtomy 3/and 4/spinning, spinning speed 5000m/minute about, energy consumption and waste silk rate relatively high.
Have based on this, make the present invention
Summary of the invention
Technical problem to be solved by this invention is: a kind of method providing melt direct spinning single head High-speed machining polyester industrial filament, realizes the object of production fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament of low energy consumption, high finished product rate.
For achieving the above object, the technical scheme taked of the present invention is as follows:
The production method of fused mass directly spinning HMLS Polyester industrial filament, comprises the following steps successively:
(1) melt liquid-phase tackifying: the low sticky melt being 0.65-0.70dl/g by polycondensation gained viscosity is delivered directly in vertical liquid-phase tackifying still and carries out the polymerization of melt liquid-phase tackifying, the top of low sticky melt self-supporting liquid-phase tackifying still enters, under Action of Gravity Field, natural film forming flows down;
(2) melt direct spinning: high viscosity polyester melt Conveying, to each spinning station, enters spinning manifold, melt is sprayed by spinnerets after metering, filtration, then after ring quenching, boundling oils, and enters spinning shaft;
(3) drawing and heat-setting: carry out two-stage stretching, and relaxation heat setting;
(4) coiling and molding: through the fiber of step (3) after network processes, coiling and molding, obtained product.
For realizing better processing effect, arranging further of the technical program is as follows:
In step (1), described liquid-phase tackifying carries out in the film formation reaction still of vertical liquid-phase tackifying still, and reaction temperature is 275 ~ 285 DEG C, 90 ~ 110 minutes reaction time, and the melt viscosity that thickening obtains is that 0.90-1.05dl/g, b value is less than 4.
In step (2), spinning adopts 4/and 6/spinning, and after the pump of measuring pump, pressure is 15 ~ 25MPa, and filtering accuracy is 15 ~ 20 μm, and the diameter of spinnerets is 200 ~ 250mm, and spinning temperature is 290 ~ 300 DEG C; Slow cooling heating adopts slow cooling heating collar, and the diameter of slow cooling heating collar is 200 ~ 260mm, and height is 50 ~ 100mm, and slow cooling heating-up temperature is 300 ~ 350 DEG C; Be provided with filtering material in annular air blower, filtering material adopts the bondedfibre fabric cylindrical structure of stacked winding, and ring blowing temperature is 50 ~ 70 DEG C, and humidity is 60 ~ 70%, and leeway is 15 ~ 25Pa; Spinning shaft is square, and its tube wall is perforated plate construction.
In step (3), two-stage stretches and comprises one-level stretching and secondary drawing, and one-level draw ratio is 1.2 ~ 1.5, and secondary drawing ratio is 1.3 ~ 1.8, and the temperature of drawing process is 90 ~ 100 DEG C, and total drawing ratio is 1.8 ~ 2.5; The temperature of relaxation heat setting is 230 ~ 260 DEG C, and total relaxation rate is 2.5-3.0%.
In step (4), winding speed is 5200 ~ 6500 ms/min.
Operation principle and the beneficial effect of technical solution of the present invention are as follows:
Present invention employs the vertical viscosity-increasing reactor with independent intellectual property right, melt enters from top and distributes, flowed down by gravity nature film forming, without the need to Powered Propulsion, the Small molecular product that polycondensation produces is removed by vacuum suction, melt first in first out, ensure that high sticky melt has consistent reaction condition and the time of staying in the reactor.The polymeric reaction temperature in liquid-phase tackifying stage controls at 275 DEG C-285 DEG C, and the reaction time controls at 90-110 minute.Adopt above-mentioned process conditions, the generation of side reaction in high temperature thickening course of reaction can be suppressed, ensure that melt form and aspect are good, meanwhile, also effectively can improve melt viscosity, Reaction time shorten, maintain Large Copacity long-term operation, export the sticky melt of high-quality polyester height, the melt viscosity after thickening can reach more than 0.90-1.05 dl/g, melt b value is less than 4, can meet the demand of terylene industrial yarn spinning.
The present invention compared with prior art has the following advantages:
1, with high-viscosity polyester melt for raw material, large discharge directly spins HMLS Polyester industrial yarns, the spinning fiber number of single head can reach for 2000 dawn, the fracture strength of fiber is greater than 7.0cN/dtex, spinning technique speed can reach 6500 ms/min, compared with existing HMLS Polyester industrial filament production process, not only melt viscosity improves greatly, the qualities such as melt form and aspect are better, under the prerequisite that melt and fiber quality are protected, to shorten the reaction time, production efficiency improves greatly.
2, the filtering material of annular air blower adopts nonwoven material, and stacked being wrapped in axially is dried on endless belt, and thickness is 15-25mm, both ensure that wind speed profile was even, and has also been conducive to the air filtration in cooling procedure, and is beneficial to fiber sizing.
3, spinning shaft is designed to square tube wall and fenced by multiwell plate format, and the spinning shaft of loose structure, makes inside and outside air balance, and is easy to the heat exchanging strand.
4, owing to being melt direct spinning, flow not by spinning screw spinning limits, thus, in technical solution of the present invention, spinning machine adopts 4/and 6/, the high modulus low shrinkage polyester industrial filament that this method is produced, constant product quality, production efficiency is high, improves the output of unit interval, reduces energy consumption and production cost.
The product of employing obtained by technical solution of the present invention can as excellent materials such as tire cord, geotechnological barrier, polyester cords.
Below in conjunction with detailed description of the invention, technical solution of the present invention is further elaborated.
Detailed description of the invention
embodiment 1
One, technological parameter is as follows:
Equipment: LSP liquid phase polymerization equipment; Spinning equipment; Stretching and winding equipment.
Product specification: 1670dtex/360f.
Raw material: viscosity 1.05dl/g after glossy polyester melt thickening; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%.
Liquid phase polymerization temperature: 278-285 DEG C.
Spinning temperature: 290 DEG C.
Slow cooling heating-up temperature: 340 DEG C.
Dosing pump is for amount: 867g/min.
Ring quenching parameter
Leeway: 20Pa; Humidity: 65%; Wind-warm syndrome: 60 DEG C.
Stretching condition (two-stage stretching)
One-level draw ratio: 1.3
Total draw ratio: 1.97
Draw roll speed m/min temperature DEG C
GR1 2748
GR2 3572 98
GR3 5413 250
GR4 5413 255
GR5 5413 254
GR6 5310 130
Relaxation rate: 2.93%.
Winding speed: 5200m/min.
Spinning oil: Japan produces, TERON E-7502, compound concentration 17%.
Network device pressure: first network 0.2MPa,
Second network 0.2MPa,
3rd network 0.55MPa
Two, concrete technology step:
1) process high-viscosity polyester melt: first by base polyester melt (low sticky melt) by Cemented filling to liquid phase polymerizer thickening once again; reaction temperature is 278 DEG C; 90 minutes reaction time; under the protection of high vacuum, melt improves viscosity by film apparatus, and the ethylene glycol that reaction produces and other side reaction thing are by vacuum sucking-off.Melt viscosity brings up to 1.05dl/g from 0.655 dl/g;
2) direct fabrics: the polyester fondant after being polymerized by liquid-phase tackifying is delivered to spinning manifold by melt house steward, enter after filament spinning component through measuring pump again and extrude from spinnerets, the diameter of spinnerets is 240mm, heated by slow cooling heating collar, slow cooling heating-up temperature is 340 DEG C, the diameter of slow cooling heating collar is 260mm, height is 100mm, again by annular air blower cooling forming, blowing temperature is at 60 DEG C, humidity is 65%, leeway is 20Pa, the filtering material of annular air blower adopts non-woven material, and be stackedly wrapped on the blowing ring of annular air blower, then spinning shaft is entered, spinning shaft is designed to square, tube wall is made up of porous plate, every synnema has the porous spinning shaft of a square tube type, makes inside and outside air balance, and is easy to the heat exchanging strand,
3) stretching and winding: at 4/, 4/line, single head fiber number is 1670dtex, spinning speed 2600 ~ 3600 ms/min; Oil on silk surface, adopt two-stage high-speed stretch, under heating-up temperature 90 ~ 100 DEG C of conditions, stretch, total draw ratio is 1.97; Be under the condition of 250 ~ 256 DEG C in temperature, carry out high temperature, relaxation heat setting; And in the scope of process speed 5200 ms/min coiling and molding, obtained finished product.
The High Modulus And Low Shrinkage polyester industrial filament that the present embodiment is produced, line density is 1670dtex, fracture strength is greater than 7.0cN/dtex, the coefficient of variation is less than 4.5%, elongation at break 12 ± 2%, dry-hot shrinkage 3.5% ± 0.8 (177oC × 1min with0.05g/d), initial modulus is greater than 95cN/dtex.
embodiment 2
One, technological parameter is as follows:
Equipment: LSP liquid phase polymerization equipment; Spinning equipment; Stretching and winding equipment.
Product specification: 1440dtex/360f
Raw material: viscosity 1.05dl/g after glossy polyester melt thickening; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%
Liquid phase polymerization temperature: 278 ~ 285 DEG C
Spinning temperature: 290 DEG C
Slow cooling heating-up temperature: 340 DEG C
Pump is for amount: 751g/min
Ring quenching parameter
Leeway: 18Pa; Humidity: 65%; Wind-warm syndrome: 60 DEG C
Stretching condition (two-stage stretching)
One-level draw ratio: 1.3
Total draw ratio: 1.96
Draw roll speed m/min temperature DEG C
GR1 2780
GR2 3614 98
GR3 5449 250
GR4 5449 255
GR5 5449 254
GR6 5280 130
Relaxation rate: 3.21%
Winding speed: 5200m/min
Spinning oil: Japan produces, TERON E-7502 compound concentration 17%
Network device pressure: first network 0.2MPa,
Second network 0.2MPa
3rd network 0.55MPa
Two, concrete technology step:
1) process high-viscosity polyester melt: first by base polyester by Cemented filling to liquid phase polymerizer thickening once again; reaction temperature is 278 DEG C; 90 minutes reaction time; under the protection of high vacuum, melt improves viscosity by film apparatus, and the ethylene glycol that reaction produces and other side reaction thing are by vacuum sucking-off.Melt viscosity brings up to 1.05dl/g from 0.655;
2) direct fabrics: the polyester fondant after liquid phase polymerization is delivered to spinning manifold by melt house steward, enter after filament spinning component through measuring pump again and extrude from spinnerets, the diameter of spinnerets is 220mm, heated by slow cooling heating collar, slow cooling heating-up temperature is 340 DEG C, the diameter of slow cooling heating collar is 240mm, height is 100mm, again by annular air blower cooling forming, blowing temperature is at 60 DEG C, humidity is 65%, leeway is 18Pa, the filtering material of annular air blower adopts non-woven material, and stacked being wrapped in is dried on ring, then spinning shaft is entered, spinning shaft is designed to square, tube wall is made up of porous plate, every synnema has the porous spinning shaft of a square tube type, makes inside and outside air balance, and is easy to the heat exchanging strand,
3) stretching and winding: at 6/, on the spinning machine of 3/line, single head fiber number is 1440dtex, spinning speed 2600 ~ 3600 ms/min; Oil on silk surface, carry out the two-stage high-speed stretch in above-mentioned technological parameter, under heating-up temperature 90 ~ 100 DEG C of conditions, stretch, total draw ratio is 1.96; Be under the condition of 250 ~ 256 DEG C in temperature, carry out high temperature, relaxation heat setting; And in the scope of process speed 5200 ms/min coiling and molding, obtained finished product.
The High Modulus And Low Shrinkage polyester industrial filament that the present embodiment is produced, line density 1440dtex, fracture strength is greater than 7.0cN/dtex, the coefficient of variation is less than 4.5%, elongation at break 12 ± 2%, dry-hot shrinkage 3.5% ± 0.8 (177oC × 1min with0.05g/d), initial modulus is greater than 95cN/dtex.
embodiment 3
One, technological parameter is as follows:
Equipment: LSP liquid phase polymerization equipment; Spinning equipment; Stretching and winding equipment.
Product specification: 1110dtex/240f
Raw material: viscosity 1.05dl/g after glossy polyester melt thickening; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%
Liquid phase polymerization temperature: 278-285 DEG C
Spinning temperature: 290 DEG C
Slow cooling heating-up temperature: 340 DEG C
Pump is for amount: 644g/min
Ring quenching parameter
Leeway: 17Pa; Humidity: 65%; Wind-warm syndrome: 60 DEG C
Stretching condition (two-stage stretching)
One-level draw ratio: 1.3
Total draw ratio: 2.06
Draw roll speed m/min temperature DEG C
GR1 2935
GR2 3816 90
GR3 6046 240
GR4 6046 254
GR5 6046 254
GR6 5880 130
Relaxation rate: 2.84%
Winding speed: 5800m/min
Spinning oil: Japan produces, TERON E-7502
Network device pressure: first network 0.2MPa,
Second network 0.2MPa
3rd network 0.55MPa
Two, concrete technology step:
1) process high-viscosity polyester melt: first by base polyester by Cemented filling to liquid phase polymerizer thickening once again; reaction temperature is 278 DEG C; 90 minutes reaction time; under the protection of high vacuum, melt improves viscosity by film apparatus, and the ethylene glycol that reaction produces and other side reaction thing are by vacuum sucking-off.Melt viscosity brings up to 1.05dl/g from 0.655;
2) direct fabrics: the polyester fondant after liquid phase polymerization is delivered to spinning manifold by melt house steward, enter after filament spinning component through measuring pump again and extrude from spinnerets, the diameter of spinnerets is 220mm, heated by slow cooling heating collar, slow cooling heating-up temperature is 340 DEG C, the diameter of slow cooling heating collar is 240mm, height is 100mm, again by annular air blower cooling forming, blowing temperature is at 60 DEG C, humidity is 65%, leeway is 17Pa, the filtering material of annular air blower adopts non-woven material, and stacked being wrapped in is dried on ring, then spinning shaft is entered, spinning shaft is designed to square, tube wall is made up of porous plate, every synnema has the porous spinning shaft of a square tube type, makes inside and outside air balance, and is easy to the heat exchanging strand,
3) stretching and winding: at 6/, 3/line, single head fiber number is 1110dtex, spinning speed 2600 ~ 3600 ms/min; Oil on silk surface, two-stage high-speed stretch, under heating-up temperature 90 ~ 100 DEG C of conditions, stretch, total draw ratio is 2.06; Be under the condition of 250 ~ 256 DEG C in temperature, carry out high temperature, relaxation heat setting; And in the scope of process speed 5800 ms/min coiling and molding, obtained finished product.
The High Modulus And Low Shrinkage polyester industrial filament that the present embodiment is produced, line density 1110dtex, fracture strength is greater than 7.0cN/dtex, the coefficient of variation is less than 4.5%, elongation at break 12 ± 2%, dry-hot shrinkage 3.5% ± 0.8 (177oC × 1min with0.05g/d), initial modulus is greater than 95cN/dtex.
embodiment 4
The technological parameter of the present embodiment is as follows:
Equipment: LSP liquid phase polymerization equipment; Spinning equipment; Stretching and winding equipment.
Product specification: 1670dtex/360f.
Raw material: viscosity 1.05dl/g after glossy polyester melt thickening; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%.
The reaction temperature of liquid-phase tackifying is 275 DEG C, 110 minutes reaction time, and the melt viscosity that thickening obtains is that 1.05dl/g, b value is less than 4.
Spinning adopts 4/, and after the pump of measuring pump, pressure is 20MPa, and filtering accuracy is 20 μm, and the diameter of spinnerets is 240mm, and spinning temperature is 290 DEG C; The diameter of slow cooling heating collar is 250mm, and height is 100mm, and slow cooling heating-up temperature is 350 DEG C; In annular air blower, ring blowing temperature is 70 DEG C, and humidity is 60%, and leeway is 20Pa; Oil applying rate is 0.4% ± 0.2.
Two-stage stretches and comprises one-level stretching and secondary drawing, and one-level draw ratio is 1.2, and secondary drawing ratio is 1.8, and the temperature of drawing process is 100 DEG C, and total drawing ratio is 2.16.
The temperature of relaxation heat setting is 250 DEG C, and total relaxation rate is 3.0%.
Other technical process are identical with embodiment 1.
embodiment 5
The technological parameter of the present embodiment is as follows:
Equipment: LSP liquid phase polymerization equipment; Spinning equipment; Stretching and winding equipment.
Product specification: 1440dtex/360f
Raw material: viscosity 1.05dl/g after glossy polyester melt thickening; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%
The reaction temperature of liquid-phase tackifying is 285 DEG C, 90 minutes reaction time, and the melt viscosity that thickening obtains is that 1.05dl/g, b value is less than 4.
Spinning adopts 6/, 3/line, and after the pump of measuring pump, pressure is 25MPa, and filtering accuracy is 15 μm, and the diameter of spinnerets is 220mm, and spinning temperature is 290 DEG C; The diameter of slow cooling heating collar is 200mm, and height is 50mm, and slow cooling heating-up temperature is 300 DEG C; In annular air blower, ring blowing temperature is 60 DEG C, and humidity is 70%, and leeway is 15Pa; Oil applying rate is 0.4% ± 0.2.
Two-stage stretches and comprises one-level stretching and secondary drawing, and one-level draw ratio is 1.5, and secondary drawing ratio is 1.3, and the temperature of drawing process is 90 DEG C, and total drawing ratio is 1.95.
The temperature of relaxation heat setting is 230 DEG C, and total relaxation rate is 2.5%.
Other technical process are identical with embodiment 2.
embodiment 6
The technological parameter of the present embodiment is as follows:
Equipment: LSP liquid phase polymerization equipment; Spinning equipment; Stretching and winding equipment.
Product specification: 1110dtex/240f
Raw material: viscosity 1.02dl/g after glossy polyester melt thickening; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%
The reaction temperature of liquid-phase tackifying is 285 DEG C, 100 minutes reaction time, and the melt viscosity that thickening obtains is that 1.02dl/g, b value is less than 4.
Spinning adopts 6/, 3/line, and after the pump of measuring pump, pressure is 20MPa, and filtering accuracy is 18 μm, and the diameter of spinnerets is 220mm, and spinning temperature is 290 DEG C; The diameter of slow cooling heating collar is 240mm, and height is 80mm, and slow cooling heating-up temperature is 330 DEG C; In annular air blower, ring blowing temperature is 60 DEG C, and humidity is 65%, and leeway is 20Pa; Oil applying rate is 0.4% ± 0.2.
Two-stage stretches and comprises one-level stretching and secondary drawing, and one-level draw ratio is 1.4, and secondary drawing ratio is 1.5, and the temperature of drawing process is 95 DEG C, and total drawing ratio is 2.1.
The temperature of relaxation heat setting is 250 DEG C, and total relaxation rate is 2.8%.
Other technical process are identical with embodiment 3.
Above-mentioned six embodiment product quality indicators are in table 1:
Under table 1 different technology conditions, the quality index of products obtained therefrom
Table 2 cord fabric thread product processing quality data (1110dtex/240f × 2)
The industrial HLMS terylene thread product using this technology to produce, can adapt to the application such as automobile tire cord fabric thread, senior geotechnological barrier, conveyer belt, cotton rope, fully demonstrate the high-modulus of polyester industrial filament and the performance of lower shrinkage.
Claims (3)
1. the production method of fused mass directly spinning HMLS Polyester industrial filament, is characterized in that, comprises the steps:
(1) melt thickening: low for polycondensation gained sticky melt is delivered directly in vertical liquid-phase tackifying still and carries out the polymerization of melt liquid-phase tackifying, the top of low sticky melt self-supporting liquid-phase tackifying still enters, and under Action of Gravity Field, natural film forming flows down,
Wherein, the low sticky melt of described liquid-phase tackifying to be viscosity polycondensation obtained be 0.65-0.70dl/g carries out thickening in the film formation reaction still of vertical liquid-phase tackifying still, reaction temperature is 275 ~ 285 DEG C, 90 ~ 110 minutes reaction time, the melt viscosity that thickening obtains is that 0.90-1.05dl/g, b value is less than 4;
(2) melt direct spinning: high viscosity polyester melt Conveying is to each spinning station, enter spinning manifold, melt is sprayed by spinnerets after metering, filtration, then after ring quenching, boundling oils, and enters spinning shaft, spinning adopts 4/and 6/spinning, after the pump of measuring pump, pressure is 15 ~ 25MPa, and filtering accuracy is 15 ~ 20 μm, and the diameter of spinnerets is 200 ~ 250mm, spinning temperature is 290 ~ 300 DEG C
Wherein, slow cooling heating adopts slow cooling heating collar, and the diameter of slow cooling heating collar is 200 ~ 260mm, and height is 50 ~ 100mm, and slow cooling heating-up temperature is 300 ~ 350 DEG C; In annular air blower, ring blowing temperature is 50 ~ 70 DEG C, and humidity is 60 ~ 70%, and leeway is 15 ~ 25Pa; Oil and adopt oil tanker to oil, oil tanker is arranged at below spinning shaft, and oil applying rate is 0.4% ± 0.2;
(3) drawing and heat-setting: carry out two-stage stretching, two-stage stretches and comprises one-level stretching and secondary drawing, one-level draw ratio is 1.2 ~ 1.5, secondary drawing ratio is 1.3 ~ 1.8, the temperature of drawing process is 90 ~ 100 DEG C, and total drawing ratio is 1.8-2.5, relaxation heat setting again after two-stage stretches, the temperature of relaxation heat setting is 230 ~ 260 DEG C, and total relaxation rate is 2.5-3.0%;
(4) coiling and molding: through the fiber of step (3) after network processes, coiling and molding, obtained product.
2. the production method of fused mass directly spinning HMLS Polyester industrial filament according to claim 1, is characterized in that: be provided with filtering material in described annular air blower, and filtering material adopts the bondedfibre fabric cylindrical structure of stacked winding.
3. the production method of fused mass directly spinning HMLS Polyester industrial filament according to claim 1, it is characterized in that: in step (2), spinning shaft is square, and its tube wall is perforated plate construction.
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| CN103436973B (en) * | 2013-09-12 | 2015-12-23 | 艾艾精密工业输送系统（上海）股份有限公司 | A kind of monofilament polyester and its preparation method and application |
| CN103643309A (en) * | 2013-11-30 | 2014-03-19 | 常熟涤纶有限公司 | Manufacturing method of melt direct spinning polyester activation industrial yarns |
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| CN105862152A (en) * | 2016-06-06 | 2016-08-17 | 浙江尤夫高新纤维股份有限公司 | Production method for high-speed spinning low-stretching high-modulus low-shrinkage polyester industrial filaments |
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| CN108570718A (en) * | 2017-03-13 | 2018-09-25 | 浙江佳宝新纤维集团有限公司 | The preparation method of high-strength flatness low boiling water polyester filament is directly spun in melting |
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