CN109930240B - Filament and preparation method thereof - Google Patents
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- CN109930240B CN109930240B CN201810527431.1A CN201810527431A CN109930240B CN 109930240 B CN109930240 B CN 109930240B CN 201810527431 A CN201810527431 A CN 201810527431A CN 109930240 B CN109930240 B CN 109930240B
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Abstract
The invention provides a filament and a preparation method thereof. The filament comprises 85-98 parts by weight of polyester and 2-15 parts by weight of polyamide, wherein the polyester is selected from at least one of polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate and modified polyethylene terephthalate, and the polyamide is selected from at least one of polyamide 6, polyamide 5X and polyamide 6X; wherein the intrinsic viscosity of the polyester is 0.9-1.5dL/g, and the relative viscosity of the polyamide is 3.2-4.0. The preparation method of the filament comprises the following steps: 1) preparing the polyester and the polyamide into a mixed melt; 2) preparing the mixed melt into primary silk; 3) and cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn. The filament of the invention has high strength, good hygroscopicity, wear resistance and dyeability.
Description
Technical Field
The invention belongs to the technical field of fibers, and particularly relates to a filament and a preparation method thereof.
Background
The polyester filament has the advantages of high strength, large modulus, solvent resistance, heat resistance, fatigue resistance and the like, and is widely applied to the aspects of civil and industrial materials. However, because polyester macromolecular chains are arranged closely, the crystallinity and the orientation degree are high, and polar groups are lacked on the molecular chains, the prepared filaments have the defects of poor hygroscopicity and dyeing property, easy generation of static electricity, easy pilling of fabrics, poor wear resistance and the like; in addition, polyester filaments are generally dyed by disperse dyes and need to be dyed under high-temperature and high-pressure conditions, so that the operation is dangerous, the requirements on dyeing equipment are high, and energy is wasted.
In order to overcome the defects of the polyester filament, the polyester filament is modified mainly by physical and chemical methods at present. Wherein, the chemical method comprises copolymerization, surface treatment and the like, and the method improves the performance of the fiber by changing the chemical structure of the original macromolecules of the polyester; the physical method is to achieve the purpose of improving the fiber performance by changing the morphological structure of the fiber under the condition of not changing the chemical structure of the polyester macromolecule, and comprises composite spinning, blended spinning, anisotropic spinning, fiber mixing, interweaving and the like, thereby preparing the fiber which is easy to dye, highly hygroscopic, antistatic and soft.
The patent with publication number CN103757745B discloses a polyester blend fiber and a preparation method thereof, modified polyester and polyamide are blended and spun, wherein the modified polyester is chemically modified in polymerization, the molecular chain structure is seriously damaged, in addition, the selected blend material is polyamide 6 and polyamide 66, and the blend fiber is dyed by acid dye under the conditions of normal temperature and normal pressure to prepare civil common strength filaments. The polyester blended fiber prepared by the method has low strength, and in addition, the blended fiber is prepared by adopting a copolymerization and blending mode, so that the operation is complicated, and the investment of production cost is increased.
The patent with publication number CN105040156A discloses a blend fiber and a preparation method thereof and a fabric containing the blend fiber, wherein the blend fiber comprises 1-40 parts by weight of polyamide A (viscosity number is 70-180mL/g, namely relative viscosity is 1.7-3.1) and 60-99 parts by weight of polyester (intrinsic viscosity is 0.7-0.9dL/g), the blend fiber is subjected to blend spinning by adopting a conventional viscosity slice and conventional POY, FDY, UDY and short fiber spinning processes, the breaking strength of the blend fiber is 1.5-5.5cN/dtex, and the blend fiber belongs to common strong civil filaments and cannot meet the requirements of high-strength filaments.
Disclosure of Invention
The invention provides a filament and a preparation method thereof, and the filament prepared by the preparation method has high strength and good hygroscopicity, wear resistance and dyeability.
The invention provides a filament, comprising 85-98 parts by weight of polyester and 2-15 parts by weight of polyamide, wherein the polyester is selected from at least one of polyethylene terephthalate, polypropylene terephthalate, polybutylene terephthalate and modified polyethylene terephthalate, and the polyamide is selected from at least one of polyamide 6, polyamide 5X and polyamide 6X; wherein the intrinsic viscosity of the polyester is 0.9-1.5dL/g, and the relative viscosity of the polyamide is 3.2-4.0.
In order to overcome the defects of difficult dyeing, poor moisture absorption and the like of polyester filaments, the polyamide resin with the melting point and the crystallization temperature close to those of polyester is selected for blending spinning, so that the regularity of the molecular weight of the polyester is disturbed, the proportion of an amorphous area is increased, the moisture absorption performance of fibers is improved, and the aim of dyeing the disperse dye under the normal pressure condition is fulfilled.
In the present invention, the polyester is preferably polyethylene terephthalate. The polyethylene terephthalate belongs to crystalline high polymer, and can adopt a melt spinning method to prepare fibers.
In the present invention, the polyamide is preferably polyamide 5X, and the polyamide 5X may be at least one selected from the group consisting of polyamide 56, polyamide 510, and polyamide 512.
Further, in the filament of the present invention, the content of the polyester is preferably 86 to 93 parts by weight, more preferably 88 to 92 parts by weight; the content of the polyamide is preferably 4 to 13 parts by weight, and more preferably 6 to 10 parts by weight.
Further, the intrinsic viscosity of the polyester is preferably 1.0 to 1.4dL/g, more preferably 1.1 to 1.3dL/g, and further preferably 1.15 to 1.25 dL/g; the relative viscosity of the polyamide is preferably 3.3 to 3.9, more preferably 3.4 to 3.8, and still more preferably 3.5 to 3.7.
In the present invention, the polyamide 5X may be polymerized from raw materials including monomers including 1, 5-pentanediamine and a dibasic acid. Wherein, the dibasic acid can be at least one of aliphatic dicarboxylic acid, alicyclic dicarboxylic acid and aromatic dicarboxylic acid; specifically, the dibasic acid may be selected from at least one of C6-20 aliphatic dibasic acids; the number of carbon atoms of the dibasic acid is preferably 8 to 20, more preferably 10 to 16.
Specifically, the dibasic acid is at least one selected from adipic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, hexadecanedioic acid, heptadecanedioic acid, octadecanedioic acid, maleic acid and Δ 9-1, 18-octadecenedioic acid.
Further, the monomer may further include a comonomer, and the comonomer may be selected from at least one of ethylenediamine, hexamethylenediamine, cyclohexanediamine, xylylenediamine, 6-aminocaproic acid, 11-aminoundecanoic acid, 12-aminododecanoic acid, p-aminomethylbenzoic acid, caprolactam, and ω -laurolactam.
In addition, the raw material may further include an additive selected from at least one of a matting agent, a flame retardant, an antioxidant, an ultraviolet absorber, an infrared absorber, a crystal nucleating agent, a fluorescent whitening agent, and an antistatic agent. Wherein the mass content of the additive in the raw material can be 0.001-10 wt%.
The invention does not strictly limit the preparation method of the 1, 5-pentanediamine and/or the dibasic acid; preferably, the 1, 5-pentanediamine and/or the dibasic acid can be prepared from bio-based raw materials by a fermentation method or an enzymatic conversion method, and the materials which are not petroleum-based (i.e. bio-based) are adopted, so that the pollution is not generated greatly, and the environment is protected.
The filaments of the invention satisfy the following conditions:
the breaking strength of the filament is 6.0-10.0cN/dtex, preferably 6.5-9.5cN/dtex, more preferably 7.0-9.0cN/dtex, and even more preferably 7.5-8.5 cN/dtex;
the dry heat shrinkage of the filament is 2.0-8.0%, preferably 3.0-7.0%, and more preferably 4.0-6.0%;
the boiling water shrinkage of the filament is 2.0-8.0%, preferably 3.0-6.0%, and more preferably 4.0-5.0%;
the moisture regain of the filament is 0.8-2.0%, preferably 1.0-1.8%, and more preferably 1.2-1.6%;
the filament has a disperse dye uptake of 85 to 100%, preferably 88 to 97%, and more preferably 90 to 94%.
Further, the filaments of the present invention also satisfy the following conditions:
the titer of the filament is 100-3000dtex, preferably 200-2800dtex, more preferably 500-2500dtex, and still more preferably 800-1500 dtex;
the elongation at break of the filament is 10-25%, preferably 12-22%, more preferably 14-20cN/dtex, and more preferably 16-18 cN/dtex;
the filament can realize the normal-pressure dyeability of the disperse dye; specifically, the dyeing temperature of the filament may be 50 to 130 ℃, preferably 60 to 120 ℃, and more preferably 70 to 100 ℃.
The cross-sectional shape of the filament is not particularly limited in the present invention, and may be, for example, any one of a circular shape, a trilobal shape, a cross shape, a triangular shape, a hollow triangular shape, an I-shape, a T-shape, a Y-shape, a flat shape, a pentagonal shape, a hexagonal shape, an octagonal shape, an I-shape, and a dumbbell shape.
The principle that formic acid can etch polyamide but has no etching effect on polyester is utilized, formic acid treatment is carried out on the blended filament interface, and only polyester is left on the section after polyamide is etched by formic acid, so that the blended state of polyamide and polyester can be conveniently observed and analyzed.
In a polyamide/polyester blending system, polyamide is used as a disperse phase, and the particle size of the polyamide is related to various factors, including the compatibility of the polyamide and the polyester, the viscosity of a high polymer, the mass ratio of blending components, the setting of process parameters during blending, blending equipment and the like.
In the invention, the attached drawings 1 and 2 are SEM images of polyamide 56(15 wt%)/polyester blend filaments etched by formic acid, regular holes can be observed after the polyamide 56 is etched, the polyamide 56 is uniformly distributed in a blend as a disperse phase, the formed defects are few, and the improvement of the mechanical properties of the blend filaments is facilitated.
The invention also provides a preparation method of the filament, which comprises the following steps:
1) preparing the polyester and the polyamide into a mixed melt;
2) preparing the mixed melt into primary silk;
3) and cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
In the present invention, the polyester is preferably polyethylene terephthalate, and the polyamide is preferably polyamide 5X.
Specifically, step 1) may be performed in the following manner:
1-1) polymerizing 1, 5-pentanediamine with a dibasic acid to form a polyamide 5X melt; simultaneously, polymerizing terephthalic acid and ethylene glycol to form a polyethylene terephthalate melt; then, uniformly mixing the polyamide 5X melt and the polyethylene terephthalate melt in a static mixer to obtain a mixed melt; or
1-2) drying the polyamide 5X resin and heating to a molten state to form a polyamide 5X melt; meanwhile, after drying the polyethylene terephthalate resin, heating the polyethylene terephthalate resin to a molten state to form a polyethylene terephthalate melt; then, uniformly mixing the polyamide 5X melt and the polyethylene terephthalate melt in a static mixer to obtain a mixed melt; or 1-3) respectively drying the polyethylene terephthalate resin and the polyamide 5X resin, uniformly mixing the dried polyethylene terephthalate resin and the polyamide 5X resin according to a certain proportion, and then heating and melting the mixture to obtain a mixed melt.
In step 1-1), the polymerization process of the polyamide 5X melt may comprise the steps of:
uniformly mixing 1, 5-pentanediamine, dibasic acid and water under the condition of nitrogen to prepare a salt solution of polyamide 5X, wherein the molar ratio of the 1, 5-pentanediamine to the dibasic acid is controlled to be (1-1.2): 1;
and heating the salt solution of the polyamide 5X, raising the pressure in the reaction system to 0.35-2.0MPa, exhausting, maintaining the pressure, reducing the pressure to 0-0.25MPa, and vacuumizing to the vacuum degree of-0.07-0.1 MPa to obtain the polyamide 5X melt.
In the present invention, the pressure is a gauge pressure; the temperature of the reaction system at the end of the pressure maintaining can be 230-275 ℃; the temperature of the reaction system after the pressure reduction is finished can be 245-280 ℃; the temperature after the vacuum pumping can be 260-285 ℃.
In the steps 1-2) and 1-3), the relative viscosity of the polyamide 5X resin is 3.2 to 4.0, preferably 3.3 to 3.9, more preferably 3.4 to 3.8, and still more preferably 3.5 to 3.7, wherein the relative viscosity is measured by a concentrated sulfuric acid method using an uge viscometer; the intrinsic viscosity of the polyester resin is 0.9 to 1.5dL/g, preferably 1.0 to 1.4dL/g, more preferably 1.1 to 1.3dL/g, and still more preferably 1.15 to 1.25 dL/g.
In addition, in the step 1-2) and the step 1-3), the water content of the dried polyamide 5X resin is less than or equal to 1000ppm, preferably 30-800ppm, more preferably 50-500ppm, and even more preferably 70-300 ppm; the moisture content of the polyester resin after drying is less than or equal to 100ppm, preferably 20-90ppm, more preferably 30-80ppm, and even more preferably 40-70 ppm.
In the present invention, the polyester and the polyamide may be made into a mixed melt using a screw extruder; wherein the screw extruder adopts five-zone heating, the temperature of the first zone is 180-.
Preferably, the second zone temperature is greater than the first zone temperature; the three zone temperature is greater than the first zone temperature or the second zone temperature; the temperature of the fourth zone is greater than the temperature of the first zone or the temperature of the second zone; the temperature of the fifth zone is greater than the temperature of the first zone or the temperature of the second zone.
In the present invention, step 2) may include:
spraying the mixed melt through a spinning nozzle of a spinning manifold to form the primary yarn;
wherein the temperature of the spinning manifold is 250-320 ℃, more preferably 260-310 ℃, further preferably 270-300 ℃, and further preferably 280-290 ℃; the pressure of the spinning assembly of the spinning manifold is 8-25MPa, preferably 10-23MPa, and more preferably 14-20 MPa.
In the present invention, in step 3):
the cooling may be carried out by cross-blowing at a wind speed of 0.5 to 1.2m/s, more preferably 0.6 to 0.8 m/s; the wind temperature is 15-30 ℃, preferably 20-25 ℃, and more preferably 22-23 ℃; the humidity is 60-80%, preferably 65-78%.
The stretching process comprises more than two-stage stretching, and heat setting is carried out in the second stage of stretching, wherein: the first stage stretching multiple is 2.0-4.0, the second stage stretching multiple is 1.0-2.0, the total stretching multiple is 2.0-8.0, the stretching temperature is 50-160 ℃, and the heat setting temperature is 150-240 ℃.
More specifically, the stretching process may be: feeding the oiled nascent yarn into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting.
The winding forming speed is 2000-3500m/min, preferably 2300-3200m/min, and more preferably 2600-3000 m/min.
The implementation of the invention has at least the following advantages:
1. the filament has high strength, good hygroscopicity, wear resistance and dyeability of normal pressure disperse dyes; wherein the breaking strength is 6.0-10.0cN/dtex, the dry heat shrinkage rate is 2.0-8.0%, the boiling water shrinkage rate is 2.0-8.0%, the moisture regain is 1.0-2.0%, and the disperse dye uptake is 85-100%.
2. The preparation method of the filament is simple to operate, the polyamide 5X with the melting point and the crystallization temperature close to those of polyester is selected for blending spinning, the phase separation phenomenon is not easy to occur in the melting and crystallization process, the high-strength filament can be prepared, the regularity of the molecular weight of the polyester is disturbed, the proportion of an amorphous area is increased, the moisture absorption performance of the fiber is improved, and the aim of dyeing under the conditions of normal temperature and normal pressure of the disperse dye is fulfilled.
3. The synthetic monomer of polyamide 5X resin selected for the filament is made by a biological method, is a green material, does not depend on petroleum resources and does not cause serious pollution to the environment, so that the carbon emission can be reduced, and the greenhouse effect is reduced; in addition, the preparation method of the filament can adopt the existing polyester filament production equipment, and does not need to modify the equipment, thereby saving the equipment input cost.
Drawings
FIG. 1 is an SEM image (2000 magnification) of polyamide 56(15 wt%)/polyester blend filaments after etching with formic acid;
FIG. 2 is an SEM image (magnification 5000) of polyamide 56(15 wt%)/polyester blend filaments after etching with formic acid.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The detection method of the performance parameters related to each embodiment of the invention is as follows:
1) relative viscosity:
concentrated sulfuric acid method by Ubbelohde viscometer: the dried polyamide sample (0.25. + -. 0.0002 g) was accurately weighed, dissolved by adding 50mL of concentrated sulfuric acid (96%), and the concentrated sulfuric acid flow time t0 and the polyamide sample solution flow time t were measured and recorded in a thermostatic water bath at 25 ℃.
Relative viscosity calculation formula: relative viscosity t/t0
t: polyamide sample solution flow time;
t 0: the flow time of the concentrated sulfuric acid.
2) Intrinsic viscosity:
the method is carried out according to the GB/T14901993 fiber grade polyester chip analysis method, wherein the solvent is phenol-tetrachloroethane (1: 1).
Intrinsic viscosity (unit dL/g) { [1+1.4 (t/t) { [1+ [ 1.4 ]0-1)]0.5-1}/0.7c
Wherein: t is the flow-out time of the solution; t is t0The time of solvent run-off; c is the solution concentration.
3) Fineness number:
and winding the fiber on a strand yarn length measuring instrument for 100 circles, weighing the fiber, and converting the fiber into the weight of the fiber with the length of 10000 meters to obtain the titer, unit dtex.
4) Breaking strength and elongation at break
The reference GB/T14344-: applying a pretension of 0.05 +/-0.005 cN/dtex, a holding distance of 500mm and a drawing speed of 500 mm/min.
5) Shrinkage in boiling water:
the boiling water shrinkage is measured by referring to GB/6505-: taking a section of filament, pre-tensioning by 0.05 +/-0.005 cN/dtex, marking 50.00cm at the two ends of the middle of the filament, wrapping the filament with gauze, putting the filament into boiling water for boiling for 30min, drying a sample, measuring the length between two marked points, and calculating the boiling water shrinkage by adopting the following formula:
the boiling water shrinkage rate ═ [ (initial length-length after shrinkage)/initial length ] × 100%.
6) Dry heat shrinkage:
the dry heat shrinkage was performed as specified by FZ/T50004, wherein the heat treatment temperature was 180 ℃.
7) Moisture regain:
the determination method of the moisture regain comprises the following steps: and (3) putting the washed fiber in a loose state into an oven for drying, putting the dried fiber sample in standard atmosphere specified in GB/T6529 for debugging and balancing, and humidifying for 2 h. And washing the humidity-adjusted sample, and measuring the moisture regain, wherein the moisture regain measuring method is executed according to GB/T6503, the drying temperature of an oven is 105 ℃, and the drying time is 1 h.
8)K/S：
Measured by a computer color matching instrument.
9) Dye uptake:
dye uptake (%) - (a0-At)/a0 × 100%;
and testing the concentration change of the dye solution before and after dyeing by using a spectrophotometer, wherein: a0 is the absorbance value of the characteristic absorption peak of the dye before treatment, and At is the absorbance value of the dye At the treatment time t.
10) Wear resistance:
measured by a reciprocating abrasion tester, the strength retention rate (the breaking strength after abrasion for a certain time/the breaking strength before abrasion) is multiplied by 100%; the number of times of wear-out per unit linear density is (total number of times of wear-out/linear density) × 100%.
11) SEM test
TM3000 bench-top scanning electron microscope. Defoaming the epoxy resin in advance, wherein the defoaming temperature is 40 ℃ and the defoaming time is 40min, dripping the defoamed epoxy resin into a mold provided with the blended filaments for embedding, putting the mold into a drying oven with the temperature of 60 ℃ for precuring for 2h, heating to 100 ℃ for curing for 2h, taking out the cured epoxy resin, quenching the embedded sample in liquid nitrogen, etching the cross section by formic acid, spraying gold on the cross section, placing under a scanning electron microscope, observing the cross section, and analyzing the blending form of the two phases.
Example 1
1. Preparation of the Mixed melt
Sending the polyamide 56 melt and the polyethylene terephthalate melt to a static mixer through respective melt pipelines to be uniformly mixed to obtain a mixed melt; wherein the mass ratio of the polyamide 56 melt to the polyethylene terephthalate melt is controlled to be 5: 95.
The preparation method of the polyamide 56 melt comprises the following steps: uniformly mixing 1, 5-pentanediamine, adipic acid and water under the condition of nitrogen to prepare a salt solution of polyamide 56, wherein the molar ratio of the 1, 5-pentanediamine to the adipic acid is controlled to be 1.08: 1;
heating the salt solution of the polyamide 56, increasing the pressure in the reaction system to 2.0MPa, exhausting, maintaining the pressure, reducing the pressure to 0.2MPa, and vacuumizing to-0.07 MPa to obtain a polyamide 56 melt; wherein the temperature of the reaction system is 270 ℃ after the pressure maintaining is finished, 275 ℃ after the pressure reducing is finished, and 273 ℃ after the vacuum pumping is finished.
The relative viscosity of the polyamide 56 melt was found to be 3.2 and the intrinsic viscosity of the polyethylene terephthalate melt was found to be 1.2 dL/g.
2. Preparing the raw silk
Spraying the mixed melt through a spinning nozzle of a spinning manifold to form primary raw silk; wherein the temperature of the spinning box body is 295 ℃, and the pressure of the spinning assembly is 11 MPa.
3. Preparation of filaments
And cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
Wherein the cooling mode is side-blown cooling, the wind speed is 0.8m/s, the wind temperature is 24 ℃, and the humidity of the side-blown wind is 68 percent; the winding speed was 3100 m/min.
Two-stage stretching is adopted, and the stretching process is as follows: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting; wherein the stretching multiple of the first-stage stretching is 2.5, the stretching multiple of the second-stage stretching is 1.5, the stretching temperature is 80 ℃, the total stretching multiple is 3.75, and the heat setting temperature is 220 ℃.
4. Dyeing process
Twisting, shaping, weaving, and dyeing with disperse dye at 80 deg.C, 100 deg.C, and 130 deg.C.
The results of the filament property measurements are shown in tables 1 and 2.
Example 2
1. Preparation of the Mixed melt
Respectively drying the polyamide 56 resin and the polybutylene terephthalate resin, wherein the dried polyamide 56 resin and the dried polybutylene terephthalate resin are mixed according to the mass ratio of 8: 92, uniformly mixing to obtain blended resin; wherein the relative viscosity of the polyamide 56 resin was 3.3, the intrinsic viscosity of the polybutylene terephthalate resin was 1.1dL/g, the water content of the polyamide 56 resin after drying was 180ppm, and the water content of the polybutylene terephthalate resin after drying was 80 ppm.
Heating the blended resin in a screw extruder to a molten state to form a mixed melt; wherein the screw extruder is heated in five zones, the temperature of the first zone is 248 ℃, the temperature of the second zone is 280 ℃, the temperature of the third zone is 288 ℃, the temperature of the fourth zone is 302 ℃ and the temperature of the fifth zone is 295 ℃.
2. Preparing the raw silk
Spraying the mixed melt through a spinning nozzle of a spinning manifold to form primary raw silk; wherein the temperature of the spinning manifold is 300 ℃, and the pressure of the spinning assembly is 16 MPa.
3. Preparation of filaments
And cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
Wherein the cooling mode is side-blown cooling, the wind speed is 0.6m/s, the wind temperature is 22 ℃, and the humidity of the side-blown wind is 65%; the winding speed was 2800 m/min.
Two-stage stretching is adopted, and the stretching process is as follows: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting; wherein the stretching multiple of the first-stage stretching is 3.0, the stretching multiple of the second-stage stretching is 1.4, the stretching temperature is 90 ℃, the total stretching multiple is 4.2, and the heat setting temperature is 230 ℃.
4. Dyeing process
Twisting, shaping, weaving, and dyeing with disperse dye at 80 deg.C, 100 deg.C, and 130 deg.C.
The results of the filament property measurements are shown in tables 1 and 2.
Example 3
1. Preparation of the Mixed melt
Respectively drying the polyamide 56 resin and the polyethylene terephthalate resin, wherein the dried polyamide 56 resin and the dried polyethylene terephthalate resin are mixed according to the mass ratio of 10: 90, uniformly mixing to obtain blended resin; wherein the relative viscosity of the polyamide 56 resin was 3.5, the intrinsic viscosity of the polyethylene terephthalate resin was 1.3dL/g, the water content of the polyamide 56 resin after drying was 260ppm, and the water content of the polyethylene terephthalate resin after drying was 50 ppm.
Heating the blended resin in a screw extruder to a molten state to form a mixed melt; wherein the screw extruder is heated in five zones, the temperature of the first zone is 244 ℃, the temperature of the second zone is 282 ℃, the temperature of the third zone is 292 ℃, the temperature of the fourth zone is 302 ℃, and the temperature of the fifth zone is 298 ℃.
2. Preparing the raw silk
Spraying the mixed melt through a spinning nozzle of a spinning manifold to form primary raw silk; wherein the temperature of the spinning box body is 295 ℃, and the pressure of the spinning assembly is 13 MPa.
3. Preparation of filaments
And cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
Wherein the cooling mode is side-blown cooling, the wind speed is 0.7m/s, the wind temperature is 23 ℃, and the humidity of the side-blown wind is 72 percent; the winding speed was 3100 m/min.
Two-stage stretching is adopted, and the stretching process is as follows: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting; wherein the stretching multiple of the first-stage stretching is 4.0, the stretching multiple of the second-stage stretching is 1.2, the stretching temperature is 85 ℃, the total stretching multiple is 4.8, and the heat setting temperature is 220 ℃.
4. Dyeing process
Twisting, shaping, weaving, and dyeing with disperse dye at 80 deg.C, 100 deg.C, and 130 deg.C.
The results of the filament property measurements are shown in tables 1 and 2.
Example 4
1. Preparation of the Mixed melt
Respectively drying the polyamide 512 resin and the polyethylene terephthalate resin, wherein the dried polyamide 512 resin and the dried polyethylene terephthalate resin are prepared from the following components in percentage by mass: 97 to obtain blended resin; wherein the relative viscosity of the polyamide 512 resin was 3.4, the intrinsic viscosity of the polyethylene terephthalate resin was 1.2dL/g, the water content of the polyamide 512 resin after drying was 310ppm, and the water content of the polyethylene terephthalate resin after drying was 30 ppm.
Heating the blended resin in a screw extruder to a molten state to form a mixed melt; wherein the screw extruder is heated in five zones, the temperature of the first zone is 247 ℃, the temperature of the second zone is 278 ℃, the temperature of the third zone is 295 ℃, the temperature of the fourth zone is 306 ℃, and the temperature of the fifth zone is 305 ℃.
2. Preparing the raw silk
Spraying the mixed melt through a spinning nozzle of a spinning manifold to form primary raw silk; wherein the temperature of the spinning beam is 310 ℃, and the pressure of the spinning assembly is 12 MPa.
3. Preparation of filaments
And cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
Wherein the cooling mode is side-blown cooling, the wind speed is 0.65m/s, the wind temperature is 24 ℃, and the humidity of the side-blown wind is 75 percent; the winding speed was 2700 m/min.
Two-stage stretching is adopted, and the stretching process is as follows: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting; wherein the stretching multiple of the first-stage stretching is 3.0, the stretching multiple of the second-stage stretching is 1.5, the stretching temperature is 75 ℃, the total stretching multiple is 4.5, and the heat setting temperature is 210 ℃.
4. Dyeing process
Twisting, shaping, weaving, and dyeing with disperse dye at 80 deg.C, 100 deg.C, and 130 deg.C.
The results of the filament property measurements are shown in tables 1 and 2.
Example 5
1. Preparation of the Mixed melt
Respectively drying the polyamide 510 resin and the polyethylene terephthalate resin, wherein the dried polyamide 510 resin and the dried polyethylene terephthalate resin are mixed according to the mass ratio of 5:95, uniformly mixing to obtain blended resin; wherein the relative viscosity of the polyamide 510 resin was 3.3, the intrinsic viscosity of the polyethylene terephthalate resin was 1.0dL/g, the water content of the polyamide 510 resin after drying was 110ppm, and the water content of the polyethylene terephthalate resin after drying was 40 ppm.
Heating the blended resin in a screw extruder to a molten state to form a mixed melt; wherein the screw extruder is heated in five zones, the temperature of the first zone is 250 ℃, the temperature of the second zone is 280 ℃, the temperature of the third zone is 290 ℃, the temperature of the fourth zone is 300 ℃, and the temperature of the fifth zone is 315 ℃.
2. Preparing the raw silk
Spraying the mixed melt through a spinning nozzle of a spinning manifold to form primary raw silk; wherein the temperature of the spinning beam is 308 ℃, and the pressure of the spinning assembly is 16 MPa.
3. Preparation of filaments
And cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
Wherein the cooling mode is side-blown cooling, the wind speed is 0.75m/s, the wind temperature is 25 ℃, and the humidity of the side-blown wind is 72 percent; the winding speed was 2600 m/min.
Two-stage stretching is adopted, and the stretching process is as follows: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting; wherein the stretching multiple of the first-stage stretching is 2.8, the stretching multiple of the second-stage stretching is 1.6, the stretching temperature is 65 ℃, the total stretching multiple is 4.48, and the heat setting temperature is 160 ℃.
4. Dyeing process
Twisting, shaping, weaving, and dyeing with disperse dye at 80 deg.C, 100 deg.C, and 130 deg.C.
The results of the filament property measurements are shown in tables 1 and 2.
Example 6
1. Preparation of the Mixed melt
Respectively drying the polyamide 6 resin and the polyethylene terephthalate resin, wherein the dried polyamide 6 resin and the dried polyethylene terephthalate resin are prepared from the following components in percentage by mass: 95, uniformly mixing to obtain blended resin; wherein the relative viscosity of the polyamide 6 resin was 3.2, the intrinsic viscosity of the polyethylene terephthalate resin was 1.1dL/g, the water content of the polyamide 6 resin after drying was 400ppm, and the water content of the polyethylene terephthalate resin after drying was 60 ppm.
Heating the blended resin in a screw extruder to a molten state to form a mixed melt; wherein the screw extruder is heated in five zones, the temperature of the first zone is 240 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 280 ℃, the temperature of the fourth zone is 290 ℃, and the temperature of the fifth zone is 300 ℃.
2. Preparing the raw silk
Spraying the mixed melt through a spinning nozzle of a spinning manifold to form primary raw silk; wherein the temperature of the spinning beam is 310 ℃, and the pressure of the spinning assembly is 18 MPa.
3. Preparation of filaments
And cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
Wherein the cooling mode is side-blown cooling, the wind speed is 0.68m/s, the wind temperature is 26 ℃, and the humidity of the side-blown wind is 67%; the winding speed was 2800 m/min.
Two-stage stretching is adopted, and the stretching process is as follows: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting; wherein the stretching multiple of the first-stage stretching is 3.2, the stretching multiple of the second-stage stretching is 1.5, the stretching temperature is 80 ℃, the total stretching multiple is 4.8, and the heat setting temperature is 240 ℃.
4. Dyeing process
Twisting, shaping, weaving, and dyeing with disperse dye at 80 deg.C, 100 deg.C, and 130 deg.C.
The results of the filament property measurements are shown in tables 1 and 2.
Example 7
1. Preparation of the Mixed melt
Respectively drying the polyamide 66 resin and the polyethylene terephthalate resin, wherein the dried polyamide 66 resin and the dried polyethylene terephthalate resin are mixed according to the mass ratio of 10: 90, uniformly mixing to obtain blended resin; wherein the relative viscosity of the polyamide 66 resin was 3.4, the intrinsic viscosity of the polyethylene terephthalate resin was 1.0dL/g, the water content of the polyamide 66 resin after drying was 500ppm, and the water content of the polyethylene terephthalate resin after drying was 30 ppm.
Heating the blended resin in a screw extruder to a molten state to form a mixed melt; wherein the screw extruder is heated in five zones, the temperature of the first zone is 245 ℃, the temperature of the second zone is 275 ℃, the temperature of the third zone is 285 ℃, the temperature of the fourth zone is 295 ℃, and the temperature of the fifth zone is 305 ℃.
2. Preparing the raw silk
Spraying the mixed melt through a spinning nozzle of a spinning manifold to form primary raw silk; wherein the temperature of the spinning beam is 305 ℃, and the pressure of the spinning assembly is 16 MPa.
3. Preparation of filaments
And cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
Wherein the cooling mode is side-blown cooling, the wind speed is 0.65m/s, the wind temperature is 23 ℃, and the humidity of the side-blown wind is 65%; the winding speed was 2900 m/min.
Two-stage stretching is adopted, and the stretching process is as follows: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting; wherein the stretching multiple of the first-stage stretching is 3.3, the stretching multiple of the second-stage stretching is 1.2, the stretching temperature is 85 ℃, the total stretching multiple is 3.96, and the heat setting temperature is 230 ℃.
4. Dyeing process
Twisting, shaping, weaving, and dyeing with disperse dye at 80 deg.C, 100 deg.C, and 130 deg.C.
The results of the filament property measurements are shown in tables 1 and 2.
Comparative example 1
1. Preparation of polyethylene terephthalate melt
Drying the polyethylene terephthalate resin, and heating the dried polyethylene terephthalate resin to a molten state in a screw extruder to obtain a polyethylene terephthalate melt; wherein the intrinsic viscosity of the polyethylene terephthalate resin is 1.1dL/g, and the water content of the dried polyethylene terephthalate resin is 60 ppm; the screw extruder was heated in five zones, with the temperature in the first zone being 268 ℃, the temperature in the second zone being 275 ℃, the temperature in the third zone being 295 ℃, the temperature in the fourth zone being 295 ℃ and the temperature in the fifth zone being 293 ℃.
2. Preparing the raw silk
Spraying the mixed melt through a spinning nozzle of a spinning manifold to form primary raw silk; wherein the temperature of the spinning box body is 295 ℃, and the pressure of the spinning assembly is 15 MPa.
3. Preparation of filaments
And cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
Wherein the cooling mode is side blowing cooling, the wind speed is 0.67m/s, the wind temperature is 22 ℃, the humidity of the side blowing is 63 percent, and the winding speed is 2800 m/min.
Two-stage stretching is adopted, and the stretching process is as follows: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting; wherein the stretching multiple of the first-stage stretching is 3.0, the stretching multiple of the second-stage stretching is 1.6, the stretching temperature is 95 ℃, the total stretching multiple is 4.8, and the heat setting temperature is 220 ℃.
4. Dyeing process
Twisting the filaments, shaping, weaving the stocking band, and dyeing with disperse dye at 80 deg.C, 100 deg.C, and 130 deg.C.
The results of the filament property measurements are shown in tables 1 and 2.
Comparative example 2
1. Preparation of the Mixed melt
Respectively drying the polyamide 56 resin and the polyethylene terephthalate resin, wherein the dried polyamide 56 resin and the dried polyethylene terephthalate resin are mixed according to the mass ratio of 20: 80 to obtain blended resin; wherein the relative viscosity of the polyamide 56 resin was 3.2, the intrinsic viscosity of the polyethylene terephthalate resin was 1.3dL/g, the water content of the polyamide 56 resin after drying was 260ppm, and the water content of the polyethylene terephthalate resin after drying was 50 ppm.
Heating the blended resin in a screw extruder to a molten state to form a mixed melt; wherein the screw extruder is heated in five zones, the temperature of the first zone is 244 ℃, the temperature of the second zone is 282 ℃, the temperature of the third zone is 292 ℃, the temperature of the fourth zone is 302 ℃, and the temperature of the fifth zone is 298 ℃.
2. Preparing the raw silk
Spraying the mixed melt through a spinning nozzle of a spinning manifold to form primary raw silk; wherein the temperature of the spinning box body is 295 ℃, and the pressure of the spinning assembly is 13 MPa.
3. Preparation of filaments
And cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
Wherein the cooling mode is side-blown cooling, the wind speed is 0.7m/s, the wind temperature is 23 ℃, and the humidity of the side-blown wind is 72 percent; the winding speed was 3100 m/min.
Two-stage stretching is adopted, and the stretching process is as follows: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting; wherein the stretching multiple of the first-stage stretching is 4.0, the stretching multiple of the second-stage stretching is 1.2, the stretching temperature is 85 ℃, the total stretching multiple is 4.8, and the heat setting temperature is 220 ℃.
4. Dyeing process
Twisting, shaping, weaving, and dyeing with disperse dye at 80 deg.C, 100 deg.C, and 130 deg.C.
The results of the filament property measurements are shown in tables 1 and 2.
Comparative example 3
1. Preparation of the Mixed melt
Respectively drying the polyamide 56 resin and the polyethylene terephthalate resin, wherein the dried polyamide 56 resin and the dried polyethylene terephthalate resin are mixed according to the mass ratio of 3: 97 to obtain blended resin; wherein the relative viscosity of the polyamide 56 resin was 2.34 (viscosity number 120mL/g), the intrinsic viscosity of the polyethylene terephthalate resin was 0.82dL/g, the water content of the polyamide 56 resin after drying was 80ppm, and the water content of the polyethylene terephthalate resin after drying was 40 ppm.
Heating the blended resin in a screw extruder to a molten state to form a mixed melt; wherein the screw extruder is heated in five zones, the temperature of the first zone is 245 ℃, the temperature of the second zone is 286 ℃, the temperature of the third zone is 294 ℃, the temperature of the fourth zone is 296 ℃, and the temperature of the fifth zone is 295 ℃.
2. Preparing the raw silk
Spraying the mixed melt through a spinning nozzle of a spinning manifold to form primary raw silk; wherein the temperature of the spinning box body is 295 ℃, and the pressure of the spinning assembly is 11 MPa.
3. Preparation of filaments
And cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
Wherein the cooling mode is side-blown cooling, the wind speed is 0.6m/s, the wind temperature is 24 ℃, and the humidity of the side-blown wind is 65%; the winding speed was 3200 m/min.
Two-stage stretching is adopted, and the stretching process is as follows: feeding oiled as-spun yarns into a first pair of hot rollers through a godet roller, performing primary stretching between the first pair of hot rollers and a second pair of hot rollers, performing secondary stretching between the second pair of hot rollers and a third pair of hot rollers, and performing tension heat setting; wherein the stretching multiple of the first-stage stretching is 3.0, the stretching multiple of the second-stage stretching is 1.6, the stretching temperature is 85 ℃, the total stretching multiple is 4.8, and the heat setting temperature is 180 ℃.
4. Dyeing process
Twisting, shaping, weaving, and dyeing with disperse dye at 80 deg.C, 100 deg.C, and 130 deg.C.
The results of the filament property measurements are shown in tables 1 and 2.
TABLE 1 results of measuring properties of fibers of examples and comparative examples
TABLE 2 results of measuring properties of fibers of examples and comparative examples (TABLE 1)
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (13)
1. A filament comprising 85 to 98 parts by weight of a polyester and 2 to 15 parts by weight of a polyamide, the polyester and the polyamide being produced by forming a mixed melt, the polyester being at least one selected from the group consisting of polyethylene terephthalate, polypropylene terephthalate, polybutylene terephthalate and modified polyethylene terephthalate, and the polyamide being at least one selected from the group consisting of polyamide 6, polyamide 5X and polyamide 6X; wherein the intrinsic viscosity of the polyester is 1.0-1.4dL/g, and the relative viscosity of the polyamide is 3.2-4.0.
2. A filament according to claim 1, wherein the polyamide is polyamide 5X, the polyamide 5X being selected from at least one of polyamide 56, polyamide 510 and polyamide 512.
3. A filament according to claim 1, wherein the polyamide 5X is polymerized from starting materials comprising monomers comprising 1, 5-pentanediamine and a dibasic acid selected from at least one of C6-20 aliphatic dibasic acids.
4. A filament according to claim 3, wherein the dibasic acid is selected from the group consisting of adipic acid, sebacic acid, undecanedioic acid, dodecanedioic acid, tridecanedioic acid, tetradecanedioic acid, pentadecanedioic acid, hexadecanedioic acid, heptadecanedioic acid, octadecanedioic acid and Δ ®9-at least one of 1,18 octadecenedioic acid.
5. A filament according to claim 3, wherein the monomers further comprise at least one of ethylenediamine, hexamethylenediamine, cyclohexanediamine, xylylenediamine, 6-aminocaproic acid, 11-aminoundecanoic acid, 12-aminododecanoic acid, p-aminomethylbenzoic acid, caprolactam, and ω -laurolactam.
6. A filament according to claim 3, wherein said raw material further comprises an additive selected from at least one of a delustrant, a flame retardant, an antioxidant, an ultraviolet absorber, an infrared absorber, a crystallization nucleating agent, a fluorescent whitening agent and an antistatic agent.
7. A filament according to any of the claims 1 to 6, characterized in that the breaking strength of the filament is 6.0-10.0 cN/dtex.
8. A filament according to any of claims 1 to 6, characterized in that the dry heat shrinkage of the filament is 2.0 to 8.0% and the boiling water shrinkage is 2.0 to 8.0%.
9. A filament according to any of the claims 1 to 6, characterized in that the moisture regain of the filament is 0.8-2.0%.
10. A filament according to any of the claims 1 to 6, characterized in that the filament has a disperse dye uptake of 85 to 100%.
11. A process for the preparation of a filament according to any of claims 1 to 10, comprising the steps of:
1) preparing the polyester and the polyamide into a mixed melt;
2) preparing the mixed melt into primary silk;
3) and cooling, oiling, stretching, heat setting and winding the primary yarn to obtain the filament yarn.
12. The method according to claim 11, wherein the polyester has a water content of 100ppm or less in the step 1); the water content of the polyamide is less than or equal to 1000 ppm; and preparing the polyester and the polyamide into a mixed melt by adopting a screw extruder, wherein the screw extruder is heated in five zones, the temperature of the first zone is 180-.
13. The method according to claim 11, wherein in step 3):
cooling by cross-blown air, wherein the air speed of the cross-blown air is 0.5-1.2m/s, the air temperature is 15-30 ℃, and the humidity is 60-80%;
the stretching process comprises more than two-stage stretching, and heat setting is carried out in the second stage of stretching, wherein: the first-stage stretching multiple is 2.0-4.0, the second-stage stretching multiple is 1.0-2.0, the total stretching multiple is 2.0-8.0, the stretching temperature is 50-160 ℃, and the heat setting temperature is 150-240 ℃;
the winding forming speed is 2000-3500 m/min.
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| CN111607840A (en) * | 2020-07-09 | 2020-09-01 | 福州运泉织带有限公司 | High-strength fiber for anti-cutting woven tape and preparation method thereof |
| CN112663172B (en) * | 2020-12-23 | 2023-01-10 | 常州灵达特种纤维有限公司 | High-performance polyester-polyamide blend fiber and preparation method thereof |
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