CN1537984A - Manufacturing method of high-modulus low-shrinking ferylene filament - Google Patents
Manufacturing method of high-modulus low-shrinking ferylene filament Download PDFInfo
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- CN1537984A CN1537984A CNA2003101054284A CN200310105428A CN1537984A CN 1537984 A CN1537984 A CN 1537984A CN A2003101054284 A CNA2003101054284 A CN A2003101054284A CN 200310105428 A CN200310105428 A CN 200310105428A CN 1537984 A CN1537984 A CN 1537984A
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Abstract
A high-modulus low-shrinkage polyester filament is prepared from polyester chips through pulverizing the nucleating agent, using polyester chip as carrier to prepare mother particles of nucleating agent, fusing, adding it to fused polyester chips, mixing, spinning, high-temp buffered stretching, and high-temp shape fixation in slack state. Its advantage is high spinning speed.
Description
Technical field
The present invention relates to a kind of manufacture method of polyester filament, the manufacture method of a kind of High Modulus And Low Shrinkage polyester filament of more specifically saying so.
Background technology
The High Modulus And Low Shrinkage polyester filament is a kind of newer, high-performance fiber materials, is mainly used in fields such as making radial tyre of passenger car, various high-performance rubber skeleton, coated fabric, water under high pressure tengential belt and building decoration.Suitability for industrialized production High Modulus And Low Shrinkage polyester filament has two-step method and one-step method.Two-step method is: the first step earlier makes the terylene spun filament with the polyester section, second step be with spun filament carry out the low speed super drawing, typing makes.One-step method is to make the High Modulus And Low Shrinkage polyester filament with cut into slices high speed spinning, high temperature super drawing of polyester.Because one-step method has advantages such as product quality height, profitable and occupation area of equipment are little, so one-step method is better than two step method, but because the production technology of high speed spinning, high temperature super drawing is very high to the performance requirement of equipment, speed as spinning will reach 7000 meters/minute, have only country seldom to possess the equipment of realizing one-step method production process of making in the world, therefore, one-step method applies and has a significant limitation.
Summary of the invention
The purpose of this invention is to provide a kind of manufacture method with lower spinning speed production High Modulus And Low Shrinkage polyester filament.
In order to realize above-mentioned purpose, the manufacture method of this High Modulus And Low Shrinkage polyester filament comprises the steps: successively
A, making nucleator master batch are worked into submicron order with inorganic salts nucleator, organic acid nucleator, clay class nucleator or metal oxide-type nucleator---and nanoscale is a carrier with the polyester section, makes the nucleator master batch according to a conventional method;
B, solid-phase tack producing: according to the weight portion chain extender: the polyester section is 0.5-1: 100 ratio, metal species chain extender and polyester section to be mixed, and solid-phase tack producing technology is routinely carried out solid-phase tack producing;
C, melt spinning, polyester behind the solid-phase tack producing is heated to molten condition, form polyester and melt body, the nucleator master batch is heated to molten condition, join polyester continuously and melt in the body, evenly mix, form to mix and melt body, melt in the body in this mixing, the content of calculating by weight nucleator is the 0.2%-1.0% of polyester, the spinning of body conventional method is melted in mixing, and oil on the silk fiber surface;
D, multistage high temperature are extenuated the high power after-drawing, in temperature are under 70 ℃-230 ℃ the condition, to adopt multistage high temperature to extenuate the high power after-drawing to silk fiber, and the total draw ratio that makes polyester filament is 4.8-5.2;
E, HEAT SETTING are under 220 ℃-230 ℃ the condition, the silk fiber that has carried out after-drawing to be carried out the high temperature relaxation heat setting in temperature;
F, be that coiling and molding makes finished product under 4000 meters/minute-4500 meters/minute the condition in speed.
Inorganic salts nucleator in the above-mentioned A step comprises carbonate, sulfate or silicate, the organic acid nucleator comprises benzoic sodium salt, sylvite or aryl radical thiosulfonic acid slaine, clay class nucleator comprises talcum powder, clay or pyrophillite, and the metal oxide-type nucleator comprises aluminium oxide, zinc oxide or iron oxide.
Above-mentioned metal species chain extender can be an antimonous oxide, also can be metal ion complex Ti (IV), Sn (IV), Ge (IV), Co (II), Mn (II) or Zn (II), and addition is the 0.5%-1.0% of polyester section by weight.
It is three grades that multistage high temperature in the above-mentioned D step is extenuated the high power after-drawing, the temperature of the first order is 700 ℃-18 ℃, after-drawing is compared is 1.1-1.4, partial temperature is 150 ℃-220 ℃, after-drawing is compared is 1.8-2.8, and the temperature of the third level is 210 ℃-230 ℃, after-drawing is compared is 0.8-0.95.
Initial high-modulus that the High Modulus And Low Shrinkage polyester filament has and low thermal shrinkage mechanical property are owing to become fine terylene high polymer to have high crystallization, high orientation, the structure of high regularity and lower inside residual mechanical stress.Become the high crystallization of fine terylene high polymer, high orientation texture both can to realize by the stress induced crystallization of melting high-speed spinning and high temperature high power after-drawing process, also can by increase into the crystallizing into check figure, improve relative crystallization rate of fine terylene, to realize through the after-drawing of high temperature high power again after the lower melt spinning speed spinning.Method of the present invention is to follow the latter, promptly when melt spinning, add nucleator in proportion, increase the nucleus quantity of polyester section crystallization, accelerate crystallization rate, thereby realize producing the desired high-crystallinity of High Modulus And Low Shrinkage polyester filament with lower melt spinning speed.In order to solve the stretching difficulty that causes soon because of polyester section crystallization rate, after-drawing step of the present invention adopts multistage high temperature to extenuate the high power after-drawing, the after-drawing process that makes into silk fiber is carried out by easy stages, obtains the desired high-orientation of High Modulus And Low Shrinkage polyester filament.Adopt high temperature relaxation heat setting technology, make into the silk fiber internal residual stress and reduce, performance is more stable, and percent thermal shrinkage is lower.
Granularity is a submicron order---nano level nucleator, because specific area is big, easily assembles and be difficult for dispersion, melt at polyester and to add nucleator in the body, if can not reach desired dispersed homogeneous degree, will influence the homogeneity of fiber polymer structure, and then influence the uniformity of fiber mechanics index.If directly the polyester section is mixed with nucleator, because the addition of nucleator seldom, and the both is a solid particle, be difficult to make its uniformity, for this reason, the present invention makes the higher master batch of concentration with nucleator earlier, outside the polyester spinning screw, add a sub-screw again, with sub-screw the nucleator master batch is made and melted body, with high-pressure metering pump the nucleator master batch is melted body and join polyester in proportion continuously and melt in the body, form to mix and melt body, through mixing arrangement,, body is melted in mixing mix more than thousand times again as gear pump and static mixer, after full and uniform mixing, enter the spinning pump spinning.
Adopt the manufacture method of High Modulus And Low Shrinkage polyester filament of the present invention, the High Modulus And Low Shrinkage polyester filament of producing, line density 1100dtex, fracture strength is greater than 6.98cN/dtex, fracture strength coefficient of variation 3.23C.V%, 10.2%, 170 ℃ of xeothermic contraction 3.0% in four minutes of extension at break, initial modulus is greater than 90cN/dtex.
By above narration as can be known, the manufacture method of High Modulus And Low Shrinkage polyester filament of the present invention, owing to adopted to melt in the body and added that nucleator melts body and multistage high temperature is extenuated high power after-drawing, high temperature relaxation heat setting technology to polyester, thereby can reach the High Modulus And Low Shrinkage polyester filament of standard-required with the lower spinning speed quality of production, its spinning speed is reduced to 4500 meters/minute by 7000 meters/minute, thereby reduced performance requirement to equipment, the technology difficulty of manufacturing equipment reduces, the equipment input greatly reduces, and production cost reduces greatly.
The specific embodiment
Raw material is chosen:
Polyester section is selected for use has the light terylene chips greatly, its quality index: inherent viscosity is 0.64 ± 0.015DL/g, terminal hydroxyl content≤3.0mol/T, diethylene glycol (DEG) content≤1.2%, fusing point 〉=259 ℃; Chain extender is selected metal ion complex Ti (IV) for use; Nucleator selects respectively that inorganic salts adds for use, organic acid, clay class and metal oxide-type.
Equipment:
Solid-phase tack producing: mainly contain stainless steel rotary drum, vavuum pump and heating agent boiler;
Melt spinning: mainly contain spinning screw extruder, measuring pump and filament spinning component.
Processing step:
1), solid-phase tack producing technology: be not less than in vacuum under the condition of 80Pa, drop into the chain extender of the 0.5%-1.0% of polyester section and polyester section weight, be warmed up to temperature and be not higher than 160 ℃ with rise 20 ℃-40 ℃ speed of per minute, carry out pre-crystallization, continue to be warmed up to 170 ℃-185 ℃, with polyester chip drying 2 hours-4 hours, continued to be warmed up to 220 ℃-230 ℃, insulation again 10 hours, carry out solid phase; Behind the solid phase, be cooled to 130 ℃, inflated with nitrogen is protected normal pressure, and uses for spinning in the nitrogen protection bottom discharge;
2), spinning technique: parameter sees the following form
| Parameter | Unit | Scope |
| Lateral blowing | ????m/s | ????0.3-0.45 |
| Pump is for amount | The g/s hole | ????0.3-0.5 |
| Extrusion temperature | ????℃ | ????295±5 |
| The nucleator addition | ????％ | ????0.2-1.0 |
| Total draw ratio | ????4.8-5.2 | |
| Winding speed | ????m/min | ????4000-4500 |
3), multistage high temperature is extenuated high power after-drawing, high temperature relaxation heat setting technology: parameter sees the following form
| Parameter | Unit | Scope | The after-drawing ratio |
| First pair of heat roller temperature | ????℃ | ????70-85 | First and second to hot-rolling: 1.1-1.4 second and third to hot-rolling: 1.8-2.8 third and fourth to hot-rolling: 0.8-0.95 |
| Second pair of heat roller temperature | ????℃ | ????150-180 | |
| The 3rd pair of heat roller temperature | ????℃ | ????210-220 | |
| The 4th pair of heat roller temperature | ????℃ | ????220-230 |
It is that example 1, organic acid are that example 2, clay class are that example 3, metal oxide-type are example 4 that nucleator is selected inorganic salts for use, and the granularity of nucleator is that 100 nanometers, addition respectively are 0.6% of polyester weight, and the standard of its product and actual measurement index see the following form
| Embodiment | Line density (dtex) | Fracture strength (cN/dtex) | The fracture strength coefficient of variation (C, V%) | Extension at break (%) | 170 ℃ of xeothermic contractions of 4min (%) | Initial modulus (cN/dtex) | ||||||
| Standard | Actual measurement | Standard | Actual measurement | Standard | Actual measurement | Standard | Actual measurement | Standard | Actual measurement | Standard | Actual measurement | |
| Example 1 | ?1100 | ?1100 | ≥7 | ?6.98 | ?4.0 | ?3.23 | ?10 | ?10.2 | ?3.0 | ?3.12 | ?≥90 | ?89.3 |
| Example 2 | ?1100 | ?7.32 | ?3.23 | ?10.2 | ?2.47 | ?92.5 | ||||||
| Example 3 | ?1100 | ?7.51 | ?3.23 | ?10.2 | ?3.53 | ?96.7 | ||||||
| Example 4 | ?1100 | ?7.22 | ?3.23 | ?10.2 | ?2.96 | ?92.3 | ||||||
Claims (7)
1, a kind of manufacture method of High Modulus And Low Shrinkage polyester filament is characterized in that comprising the steps: successively
A, making nucleator master batch are worked into submicron order with inorganic salts nucleator, organic acid nucleator, clay class nucleator or metal oxide-type nucleator---and nanoscale is a carrier with the polyester section, makes the nucleator master batch according to a conventional method;
B, solid-phase tack producing: according to the weight portion chain extender: the polyester section is 0.5-1: 100 ratio, metal species chain extender and polyester section to be mixed, and solid-phase tack producing technology is routinely carried out solid-phase tack producing;
C, melt spinning, polyester behind the solid-phase tack producing is heated to molten condition, form polyester and melt body, the nucleator master batch is heated to molten condition, join polyester continuously and melt in the body, evenly mix, form to mix and melt body, melt in the body in this mixing, the content of calculating by weight nucleator is the 0.2%-1.0% of polyester, the spinning of body conventional method is melted in mixing, and oil on the silk fiber surface;
D, multistage high temperature are extenuated the high power after-drawing, in temperature are under 70 ℃-230 ℃ the condition, to adopt multistage high temperature to extenuate the high power after-drawing to silk fiber, and the total draw ratio that makes polyester filament is 4.8-5.2;
E, HEAT SETTING are under 220 ℃-230 ℃ the condition, the silk fiber that has carried out after-drawing to be carried out the high temperature relaxation heat setting in temperature;
F, be that coiling and molding makes finished product under 4000 meters/minute-4500 meters/minute the condition in speed.
2, the manufacture method of High Modulus And Low Shrinkage polyester filament according to claim 1 is characterized in that the inorganic salts nucleator in the A step comprises carbonate, sulfate or silicate.
3, the manufacture method of High Modulus And Low Shrinkage polyester filament according to claim 1 is characterized in that the organic acid nucleator in the A step comprises benzoic sodium salt, sylvite or aryl radical thiosulfonic acid slaine.
4, the manufacture method of High Modulus And Low Shrinkage polyester filament according to claim 1 is characterized in that the clay class nucleator in the A step comprises talcum powder, clay or pyrophillite.
5, the manufacture method of High Modulus And Low Shrinkage polyester filament according to claim 1 is characterized in that the metal oxide-type nucleator in the A step comprises aluminium oxide, zinc oxide or iron oxide.
6,, it is characterized in that it is three grades that multistage high temperature in the D step is extenuated the high power after-drawing according to the manufacture method of claim 1,2,3,4 or 5 described High Modulus And Low Shrinkage polyester filaments.
7, the manufacture method of High Modulus And Low Shrinkage polyester filament according to claim 6, the temperature that it is characterized in that the first order is 70 ℃-180 ℃, after-drawing is compared is 1.1-1.4, partial temperature is 150 ℃-220 ℃, after-drawing is compared is 1.8-2.8, and the temperature of the third level is 210 ℃-230 ℃, after-drawing is compared is 0.8-0.95.
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| CN 200310105428 CN1243857C (en) | 2003-10-23 | 2003-10-23 | Manufacturing method of high-modulus low-shrinking ferylene filament |
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| CN 200310105428 CN1243857C (en) | 2003-10-23 | 2003-10-23 | Manufacturing method of high-modulus low-shrinking ferylene filament |
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