CN103088454A - 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 High Modulus And Low Shrinkage polyester industrial filament yarn.
Background technology
High modulus low shrinkage polyester industrial filament, be called for short the High Modulus And Low Shrinkage polyester industrial filament and be the industrial filament with higher initial modulus and lower percent thermal shrinkage, its good mechanical properties, have 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 at present production of High Modulus And Low Shrinkage polyester industrial fiber mostly is 3/of microtomies and 4/spinning, spinning speed 5000m/minute about, energy consumption and waste silk rate are relatively high.
Have based on this, make the present invention
Summary of the invention
[0005] technical problem to be solved by this invention is: a kind of method of melt direct spinning single head High-speed machining polyester industrial filament is provided, realizes the purpose of the 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 High Modulus And Low Shrinkage polyester industrial filament yarn comprises the following steps successively:
(1) melt liquid-phase tackifying: the polycondensation gained viscosity low sticking melt that is 0.65-0.70dl/g is delivered directly to carries out the polymerization of melt liquid-phase tackifying in vertical liquid-phase tackifying still, the top of low sticking melt self-supporting liquid-phase tackifying still enters, under Action of Gravity Field, natural film forming flows down;
(2) melt direct spinning: the high viscosity polyester melt Conveying enters spinning manifold to each spinning station, and melt is sprayed by spinnerets after metering, filtration, then boundling oils after the ring quenching, enters spinning shaft;
(3) drawing and heat-setting: carry out two-stage and stretch, and relaxation heat setting;
(4) coiling and molding: after network processes, coiling and molding makes product through the fiber of step (3).
For realizing better processing effect, further arranging of the technical program is as follows:
In step (1), described liquid-phase tackifying is to carry out in the film formation reaction still of vertical liquid-phase tackifying still, and reaction temperature is 275～285 ℃, and in 90～110 minutes reaction time, the melt viscosity that tackify obtains is 0.90-1.05dl/g, and the b value is less than 4.
In step (2), 4/and 6/spinning are adopted in spinning, and after the pump of measuring pump, pressure is 15～25MPa, and filtering accuracy is 15～20 μ m, and the diameter of spinnerets is 200～250mm, and spinning temperature is 290～300 ℃; Slow cooling adds thermal recovery slow cooling heating collar, and the diameter of slow cooling heating collar is 200～260mm, is highly 50～100mm, and the slow cooling heating-up temperature is 300～350 ℃; 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 ℃, 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 that one-level stretches and secondary drawing, and the one-level draw ratio is 1.2～1.5, and the secondary drawing ratio is 1.3～1.8, and the temperature of drawing process is 90～100 ℃, and total drawing ratio is 1.8～2.5; The temperature of relaxation heat setting is 230～260 ℃, and the total relaxation rate is 2.5-3.0%.
In step (4), winding speed is 5200～6500 m/mins.
Operation principle and the beneficial effect of technical solution of the present invention are as follows:
The present invention has adopted the vertical viscosity-increasing reactor with independent intellectual property right, melt enters from the top and distributes, flowed down by gravity nature film forming, need not power advances, the little molecular product that polycondensation produces is removed by vacuum suction, the melt first in first out has guaranteed that high sticking melt has consistent reaction condition and the time of staying in reactor.The polymeric reaction temperature in liquid-phase tackifying stage is controlled at 275 ℃-285 ℃, and the reaction time is controlled at 90-110 minute.Adopt above-mentioned process conditions, can suppress the generation of side reaction in high temperature tackify course of reaction, guarantee that the melt form and aspect are good, simultaneously, also can effectively improve melt viscosity, Reaction time shorten, keep large capacity long-term operation, export the high sticking melt of high-quality polyester, more than the melt viscosity after tackify can reach 0.90-1.05 dl/g, melt b value can satisfy the demand of terylene industrial yarn spinning less than 4.
The present invention compared with prior art has the following advantages:
1, take the high-viscosity polyester melt as raw material, large flow directly spins the High Modulus And Low Shrinkage polyester industry yarn, 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 m/mins, compare with existing High Modulus And Low Shrinkage polyester industrial filament yarn 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, stacked being wrapped on axial blowing endless belt, and thickness is 15-25mm, has both guaranteed that wind speed profile was even, also is conducive to the air filtration in cooling procedure, and is beneficial to the fiber typing.
3, spinning shaft is designed to square tube wall and fenced by the porous plate form, and the spinning shaft of loose structure makes inside and outside air balance, and is easy to exchange the heat of strand.
4, owing to being melt direct spinning, be not subjected to the flow restriction of spinning screw spinning, thereby, 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, has improved the output of unit interval, has reduced energy consumption and production cost.
Adopt the prepared product of technical solution of the present invention to can be used as the excellent materials such as tire cord, geotechnological barrier, polyester cord.
Below in conjunction with the specific embodiment, technical solution of the present invention is further elaborated.
The specific embodiment
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 tackify; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%.
Liquid phase polymerization temperature: 278-285 ℃.
Spinning temperature: 290 ℃.
Slow cooling heating-up temperature: 340 ℃.
Dosing pump is for amount: 867g/min.
Ring quenching parameter
Leeway: 20Pa; Humidity: 65%; Wind-warm syndrome: 60 ℃.
Stretching condition (two-stage stretching)
One-level draw ratio: 1.3
Total draw ratio: 1.97
Draw roll speed m/min temperature ℃
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,
The 3rd network 0.55MPa
Two, concrete technology step:
1) processing high-viscosity polyester melt: first base polyester melt (low sticking melt) is transported to liquid phase polymerizer tackify once again by pipeline; reaction temperature is 278 ℃; 90 minutes reaction time; melt improves viscosity by film apparatus under the protection of high vacuum, and the ethylene glycol that reaction produces and other side reaction thing are by the vacuum sucking-off.Melt viscosity is brought up to 1.05dl/g from 0.655 dl/g;
2) direct fabrics: the polyester fondant after the liquid-phase tackifying polymerization is delivered to spinning manifold by the melt house steward, after entering filament spinning component, extrudes from spinnerets measuring pump again, the diameter of spinnerets is 240mm, heated by the slow cooling heating collar, the slow cooling heating-up temperature is 340 ℃, the diameter of slow cooling heating collar is 260mm, highly 100mm, again by the annular air blower cooling forming, the blowing temperature is at 60 ℃, humidity is 65%, leeway is 20Pa, the filtering material of annular air blower adopts non-woven material, and on the stacked blowing ring that is wrapped in annular air blower, then enter spinning shaft, spinning shaft is designed to square, tube wall is made by porous plate, every synnema has the porous spinning shaft of a square tube type, makes inside and outside air balance, and is easy to exchange the heat of strand,
3) stretching and winding: at 4/, 4/line, the single head fiber number is 1670dtex, 2600～3600 m/mins of spinning speeds; Oil on the silk surface, adopt the two-stage high-speed stretch, under 90～100 ℃ of conditions of heating-up temperature, stretch, total draw ratio is 1.97; Be under the condition of 250～256 ℃, to carry out high temperature, relaxation heat setting in temperature; And in the scope of 5200 m/mins of process speeds coiling and molding, make 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 tackify; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%
Liquid phase polymerization temperature: 278～285 ℃
Spinning temperature: 290 ℃
Slow cooling heating-up temperature: 340 ℃
Pump is for amount: 751g/min
Ring quenching parameter
Leeway: 18Pa; Humidity: 65%; Wind-warm syndrome: 60 ℃
Stretching condition (two-stage stretching)
One-level draw ratio: 1.3
Total draw ratio: 1.96
Draw roll speed m/min temperature ℃
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
The 3rd network 0.55MPa
Two, concrete technology step:
1) processing high-viscosity polyester melt: first base polyester is transported to liquid phase polymerizer tackify once again by pipeline; reaction temperature is 278 ℃; 90 minutes reaction time; melt improves viscosity by film apparatus under the protection of high vacuum, and the ethylene glycol that reaction produces and other side reaction thing are by the vacuum sucking-off.Melt viscosity is brought up to 1.05dl/g from 0.655;
2) direct fabrics: the polyester fondant after liquid phase polymerization is delivered to spinning manifold by the melt house steward, after entering filament spinning component, extrudes from spinnerets measuring pump again, the diameter of spinnerets is 220mm, heated by the slow cooling heating collar, the slow cooling heating-up temperature is 340 ℃, the diameter of slow cooling heating collar is 240mm, highly 100mm, again by the annular air blower cooling forming, the blowing temperature is at 60 ℃, humidity is 65%, leeway is 18Pa, the filtering material of annular air blower adopts non-woven material, and stacked being wrapped on the blowing ring, then enter spinning shaft, spinning shaft is designed to square, tube wall is made by porous plate, every synnema has the porous spinning shaft of a square tube type, makes inside and outside air balance, and is easy to exchange the heat of strand,
3) stretching and winding: at 6/, on the spinning machine of 3/line, the single head fiber number is 1440dtex, 2600～3600 m/mins of spinning speeds; Oil on the silk surface, carry out the two-stage high-speed stretch in above-mentioned technological parameter, under 90～100 ℃ of conditions of heating-up temperature, stretch, total draw ratio is 1.96; Be under the condition of 250～256 ℃, to carry out high temperature, relaxation heat setting in temperature; And in the scope of 5200 m/mins of process speeds coiling and molding, make 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 tackify; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%
Liquid phase polymerization temperature: 278-285 ℃
Spinning temperature: 290 ℃
Slow cooling heating-up temperature: 340 ℃
Pump is for amount: 644g/min
Ring quenching parameter
Leeway: 17Pa; Humidity: 65%; Wind-warm syndrome: 60 ℃
Stretching condition (two-stage stretching)
One-level draw ratio: 1.3
Total draw ratio: 2.06
Draw roll speed m/min temperature ℃
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
The 3rd network 0.55MPa
Two, concrete technology step:
1) processing high-viscosity polyester melt: first base polyester is transported to liquid phase polymerizer tackify once again by pipeline; reaction temperature is 278 ℃; 90 minutes reaction time; melt improves viscosity by film apparatus under the protection of high vacuum, and the ethylene glycol that reaction produces and other side reaction thing are by the vacuum sucking-off.Melt viscosity is brought up to 1.05dl/g from 0.655;
2) direct fabrics: the polyester fondant after liquid phase polymerization is delivered to spinning manifold by the melt house steward, after entering filament spinning component, extrudes from spinnerets measuring pump again, the diameter of spinnerets is 220mm, heated by the slow cooling heating collar, the slow cooling heating-up temperature is 340 ℃, the diameter of slow cooling heating collar is 240mm, highly 100mm, again by the annular air blower cooling forming, the blowing temperature is at 60 ℃, humidity is 65%, leeway is 17Pa, the filtering material of annular air blower adopts non-woven material, and stacked being wrapped on the blowing ring, then enter spinning shaft, spinning shaft is designed to square, tube wall is made by porous plate, every synnema has the porous spinning shaft of a square tube type, makes inside and outside air balance, and is easy to exchange the heat of strand,
3) stretching and winding: at 6/, 3/line, the single head fiber number is 1110dtex, 2600～3600 m/mins of spinning speeds; Oil on the silk surface, the two-stage high-speed stretch under 90～100 ℃ of conditions of heating-up temperature, stretches, and total draw ratio is 2.06; Be under the condition of 250～256 ℃, to carry out high temperature, relaxation heat setting in temperature; And in the scope of 5800 m/mins of process speeds coiling and molding, make 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 tackify; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%.
The reaction temperature of liquid-phase tackifying is 275 ℃, and in 110 minutes reaction time, the melt viscosity that tackify obtains is 1.05dl/g, and the b value is less than 4.
Spinning is adopted 4/, and after the pump of measuring pump, pressure is 20MPa, and filtering accuracy is 20 μ m, and the diameter of spinnerets is 240mm, and spinning temperature is 290 ℃; The diameter of slow cooling heating collar is 250mm, is highly 100mm, and the slow cooling heating-up temperature is 350 ℃; In annular air blower, ring blowing temperature is 70 ℃, and humidity is 60%, and leeway is 20Pa; Oil applying rate is 0.4% ± 0.2.
Two-stage stretches and comprises that one-level stretches and secondary drawing, and the one-level draw ratio is 1.2, and the secondary drawing ratio is 1.8, and the temperature of drawing process is 100 ℃, and total drawing ratio is 2.16.
The temperature of relaxation heat setting is 250 ℃, and the 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 tackify; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%
The reaction temperature of liquid-phase tackifying is 285 ℃, and in 90 minutes reaction time, the melt viscosity that tackify obtains is 1.05dl/g, and the b value is less than 4.
Spinning is adopted 6/, and 3/line, after the pump of measuring pump, pressure is 25MPa, and filtering accuracy is 15 μ m, and the diameter of spinnerets is 220mm, and spinning temperature is 290 ℃; The diameter of slow cooling heating collar is 200mm, is highly 50mm, and the slow cooling heating-up temperature is 300 ℃; In annular air blower, ring blowing temperature is 60 ℃, and humidity is 70%, and leeway is 15Pa; Oil applying rate is 0.4% ± 0.2.
Two-stage stretches and comprises that one-level stretches and secondary drawing, and the one-level draw ratio is 1.5, and the secondary drawing ratio is 1.3, and the temperature of drawing process is 90 ℃, and total drawing ratio is 1.95.
The temperature of relaxation heat setting is 230 ℃, and the 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 tackify; End carboxyl-COOH≤25mol/t; Diethylene glycol (DEG)≤1.2%
The reaction temperature of liquid-phase tackifying is 285 ℃, and in 100 minutes reaction time, the melt viscosity that tackify obtains is 1.02dl/g, and the b value is less than 4.
Spinning is adopted 6/, and 3/line, after the pump of measuring pump, pressure is 20MPa, and filtering accuracy is 18 μ m, and the diameter of spinnerets is 220mm, and spinning temperature is 290 ℃; The diameter of slow cooling heating collar is 240mm, is highly 80mm, and the slow cooling heating-up temperature is 330 ℃; In annular air blower, ring blowing temperature is 60 ℃, and humidity is 65%, and leeway is 20Pa; Oil applying rate is 0.4% ± 0.2.
Two-stage stretches and comprises that one-level stretches and secondary drawing, and the one-level draw ratio is 1.4, and the secondary drawing ratio is 1.5, and the temperature of drawing process is 95 ℃, and total drawing ratio is 2.1.
The temperature of relaxation heat setting is 250 ℃, and the total relaxation rate is 2.8%.
Other technical process are identical with embodiment 3.
Above-mentioned six embodiment product quality indicators see 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 that uses present technique to produce can adapt to the application such as automobile tire cord fabric thread, senior geotechnological barrier, conveyer belt, cotton rope, has demonstrated fully high-modulus and the low performance of shrinking of polyester industrial filament.
Claims (10)
1. the production method of fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament yarn, is characterized in that, comprises the steps:
(1) melt tackify: the low sticking melt of polycondensation gained is delivered directly to carries out the polymerization of melt liquid-phase tackifying in vertical liquid-phase tackifying still, the top of low sticking melt self-supporting liquid-phase tackifying still enters, and under Action of Gravity Field, natural film forming flows down;
(2) melt direct spinning: the high viscosity polyester melt Conveying enters spinning manifold to each spinning station, and melt is sprayed by spinnerets after metering, filtration, then boundling oils after the ring quenching, enters spinning shaft;
(3) drawing and heat-setting: carry out two-stage and stretch, and relaxation heat setting;
(4) coiling and molding: after network processes, coiling and molding makes product through the fiber of step (3).
2. the production method of fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament yarn according to claim 1, it is characterized in that: in step (1), described liquid-phase tackifying is that the low sticking melt that the viscosity that polycondensation obtains is 0.65-0.70dl/g is carried out tackify in the film formation reaction still of vertical liquid-phase tackifying still, reaction temperature is 275～285 ℃, 90～110 minutes reaction time, the melt viscosity that tackify obtains is 0.90-1.05dl/g, and the b value is less than 4.
3. the production method of fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament yarn according to claim 1, it is characterized in that: in step (2), 4/and 6/spinning are adopted in spinning, after the pump of measuring pump, pressure is 15～25MPa, filtering accuracy is 15～20 μ m, the diameter of spinnerets is 200～250mm, and spinning temperature is 290～300 ℃.
4. the production method of fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament yarn according to claim 3, it is characterized in that: in step (2), slow cooling adds thermal recovery slow cooling heating collar, and the diameter of slow cooling heating collar is 200～260mm, be highly 50～100mm, the slow cooling heating-up temperature is 300～350 ℃.
5. the production method of fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament yarn according to claim 4 is characterized in that: in step (2), in annular air blower, ring blowing temperature is 50～70 ℃, and humidity is 60～70%, and leeway is 15～25Pa.
6. the production method of fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament yarn according to claim 1 or 5, it is characterized in that: be provided with filtering material in described annular air blower, filtering material adopts the bondedfibre fabric cylindrical structure of stacked winding.
7. the production method of fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament yarn according to claim 1, it is characterized in that: in step (2), spinning shaft is square, and its tube wall is perforated plate construction.
8. the production method of according to claim 1 or 7 described fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament yarns is characterized in that: in step (2), oil and adopt oil tanker to oil, oil tanker is arranged at the spinning shaft below, and oil applying rate is 0.4% ± 0.2.
9. the production method of fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament yarn according to claim 1, it is characterized in that: in step (3), two-stage stretches and comprises that one-level stretches and secondary drawing, the one-level draw ratio is 1.2～1.5, the secondary drawing ratio is 1.3～1.8, the temperature of drawing process is 90～100 ℃, and total drawing ratio is 1.8-2.5.
10. the production method of fused mass directly spinning High Modulus And Low Shrinkage polyester industrial filament yarn according to claim 1, it is characterized in that: in step (3), the temperature of relaxation heat setting is 230～260 ℃, and the total relaxation rate is 2.5-3.0%.
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