Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a novel parallel composite fiber which is soft, has good hygroscopicity, has three-dimensional curling performance and high elastic performance, and can be widely applied to the field of knitting and tatting.
The invention provides a side-by-side conjugate fiber, which comprises a first side-by-side structure and a second side-by-side structure, wherein the first side-by-side structure is polyamide 5X, and the second side-by-side structure is polyester and/or polyamide 6X.
The first polyamide 5X of the side-by-side structure is contained in an amount of 10 to 50 wt%, preferably 15 to 45 wt%, and more preferably 20 to 40 wt%; the second side-by-side polyester and/or polyamide 6X is present in an amount of 50 to 90 wt.%, preferably 55 to 85 wt.%, more preferably 60 to 80 wt.%.
The polyamide 5X can be obtained by polymerizing 1, 5-pentanediamine and dibasic acid serving as monomers, and in order to reduce environmental pollution, the 1, 5-pentanediamine and the dibasic acid can be prepared from bio-based raw materials by a fermentation method or an enzymatic conversion method.
The dibasic acid comprises C6-20 aliphatic dibasic acid, namely: the number of carbon atoms of the aliphatic dibasic acid is more than or equal to 6, preferably 8-20, and more preferably 10-16; specifically, the dibasic acids include: 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 tenAn octaene diacid.
The starting materials for the production of the polyamide 5X may contain, in addition to the abovementioned 1, 5-pentanediamine and dibasic acid, other comonomers and/or additives;
wherein the comonomers comprise: any one or more of aliphatic dicarboxylic acid, alicyclic dicarboxylic acid, aromatic dicarboxylic acid, ethylenediamine, hexamethylenediamine, cyclohexanediamine, xylylenediamine, 6-aminocaproic acid, 11-aminoundecanoic acid, 12-aminododecanoic acid, p-aminomethylbenzoic acid, caprolactam and omega-laurolactam;
the additive comprises: any one or more of a delustering agent, a flame retardant, an antioxidant, an ultraviolet absorbent, an infrared absorbent, a crystallization nucleating agent, a fluorescent brightener and an antistatic agent;
the additive accounts for 0.001-10% of the total weight of the raw materials.
Further, in the present invention, polyamide 5X is selected from any one of polyamide 56, polyamide 510, and polyamide 512; the polyester is selected from any one of polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate and modified polyester; the polyamide 6X is selected from any one of polyamide 6, polyamide 66, polyamide 610, and polyamide 612.
In the present invention, the cross-sectional shape of the side-by-side conjugate fiber is not particularly limited, and may be any 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, or a dumbbell shape.
The titer of the parallel composite fiber is 10-1000dtex, preferably 30-700dtex, more preferably 50-400dtex, more preferably 70-200dtex, and more preferably 80-150 dtex;
the breaking strength of the parallel composite fiber is 2.5-7.0cN/dtex, preferably 2.8-6.5cN/dtex, more preferably 3.2-6.0cN/dtex, and even more preferably 3.8-5.5 cN/dtex;
the elongation at break of the side-by-side conjugate fiber is 30 to 100%, preferably 40 to 90%, more preferably 50 to 80%, and still more preferably 60 to 70%;
the initial modulus of the parallel composite fiber is 20-60cN/dtex, preferably 25-55cN/dtex, more preferably 30-50cN/dtex, and more preferably 35-45 cN/dtex;
the moisture regain of the side-by-side composite fiber is 1.0-6.0%, preferably 1.5-5.5%, more preferably 2.0-5.0%, and still more preferably 2.5-4.5%;
The crimp contraction rate of the side-by-side conjugate fiber is 50 to 80%, preferably 54 to 76%, more preferably 58 to 70%, and still more preferably 62 to 65%; a modulus of crimp of 20 to 50%, preferably 23 to 47%, more preferably 28 to 42%, still more preferably 33 to 38%; the curl stability is 80 to 100%, preferably 82 to 98%, more preferably 86 to 95%, still more preferably 88 to 92%;
the untreated elastic recovery rate of the side-by-side conjugate fiber is 85 to 100%, preferably 88 to 98%, more preferably 90 to 96%, and still more preferably 92 to 94%; the elastic recovery after the treatment is 85 to 100%, preferably 87 to 98%, more preferably 91 to 96%, and still more preferably 93 to 94%.
The invention also provides a preparation method of any one of the parallel composite fibers, which comprises the following steps:
1) converging the first parallel structure melt and the second parallel structure melt in a composite spinning assembly through respective melt pipelines, and extruding through parallel composite spinneret plates to form primary yarns;
2) and cooling, oiling, stretching, heat setting and winding the raw silk to obtain the fiber.
Wherein, the polyamide 5X melt with the first parallel structure in the step 1) can be polymerized by the 1, 5-pentanediamine and the dibasic acid to obtain the polyamide 5X melt; the polyamide 5X resin can also be directly heated to a molten state to obtain a polyamide 5X melt;
The method for preparing the polyamide 5X melt by directly polymerizing 1, 5-pentanediamine and dibasic acid comprises the following steps: under the condition of nitrogen, 1, 5-pentanediamine, dicarboxylic acid and water are uniformly mixed to prepare a salt solution of polyamide 5X; wherein the molar ratio of the 1, 5-pentanediamine to the dicarboxylic acid is (1-1.2): 1; then heating the salt solution of polyamide 5X, raising the pressure in the reaction system to 0.3-2.5MPa, exhausting, maintaining the pressure, reducing the pressure to gauge pressure of 0-0.3MPa, and vacuumizing to the vacuum degree of-0.08 to-0.01 MPa to obtain a polyamide 5X melt; in the reaction process, the temperature of the reaction system is 230-275 ℃ after the pressure maintaining is finished, the temperature of the reaction system is 245-285 ℃ after the pressure reduction is finished, and the temperature after the vacuum pumping is 250-280 ℃.
In addition, in addition to the above method, the preparation of polyamide 5X can also be accomplished by adding monomers and additives, the preparation method comprising: under the condition of nitrogen, 1, 5-pentanediamine, dicarboxylic acid, caprolactam and water are uniformly mixed to prepare a salt solution of polyamide 5X, and a fluorescent whitening agent is added; wherein the molar ratio of the 1, 5-pentanediamine to the dicarboxylic acid is (1-1.08): 1, wherein the fluorescent whitening agent accounts for 0.3 wt% of the salt solution, and the caprolactam accounts for 3 wt% of the salt solution; then heating the salt solution of polyamide 5X, raising the pressure in the reaction system to 0.25-2.3MPa, exhausting, maintaining the pressure, reducing the pressure to gauge pressure of 0-0.35MPa, and vacuumizing to the vacuum degree of-0.08 to-0.01 MPa to obtain a polyamide 5X melt; in the reaction process, the temperature of the reaction system is 232-.
When the polyamide resin is selected to be directly heated to prepare the polyamide melt, the relative viscosity of 96 wt% sulfuric acid of the polyamide 5X resin is 2.0-4.0, preferably 2.2-3.6, and more preferably 2.4-3.2; the water content of the polyamide 5X resin is 50-1300ppm, preferably 200-1000ppm, more preferably 300-800ppm, and further preferably 400-700 ppm.
Further, the direct heating of the polyamide 5X resin described above is carried out in a screw extruder, which is divided into five zones of heating;
wherein the temperature of the first zone is 210-260 ℃;
the temperature of the second zone is 22-280 ℃;
the temperature of the three zones is 230-290 ℃;
the temperature of the four areas is 240-300 ℃;
the temperature of the five regions is 250-310 ℃;
preferably, the second zone temperature is greater than the first zone temperature; the three zone temperature, the four zone temperature, and/or the five zone temperature is greater than the first zone temperature and/or the second zone temperature;
likewise, the polyester of the second side-by-side structure can directly polymerize terephthalic acid and a diol selected from the group consisting of ethylene glycol, propylene glycol, and butylene glycol, respectively, to form a polyethylene terephthalate, polypropylene terephthalate, and polybutylene terephthalate melt; the polyester resin can also be directly heated to a molten state to form a melt; the polyamide 6X in the second side-by-side structure can polymerize caprolactam to form a polyamide 6 melt, and the hexamethylenediamine and the dicarboxylic acid polymerize to form a polyamide 6X melt; the polyamide 6 or polyamide 6X resin may also be heated directly to a molten state to form a melt.
Further, the direct heating of the polyester, polyamide 6 and polyamide 6X described above is also carried out in a screw extruder, which is divided into five zones of heating;
wherein the temperature of the first zone is 220-260 ℃;
the temperature of the second zone is 230-280 ℃;
the temperature of the three zones is 240-290 ℃;
the temperature of the four areas is 250-300 ℃;
the temperature of the five regions is 260-310 ℃;
preferably, the second zone temperature is greater than the first zone temperature; the three zone temperature, the four zone temperature, and/or the five zone temperature are greater than the first zone temperature and/or the second zone temperature.
When the polyester resin is selected and directly heated to prepare the polyamide melt, the inherent viscosity of the polyester is 0.6-1.2dL/g, preferably 0.7-1.1dL/g, and more preferably 0.8-1.0 dL/g; the polyester resin has a water content of 20 to 100ppm, preferably 30 to 90ppm, more preferably 40 to 80ppm, and further preferably 50 to 70 ppm.
When polyamide resin is selected to be directly heated to prepare polyamide melt, the relative viscosity of 96 wt% sulfuric acid of the polyamide 6 and polyamide 6X resin is 2.0-4.0, preferably 2.2-3.6, and more preferably 2.4-3.2; the water content of the polyamide 6 and polyamide 6X resin is 50-1300ppm, preferably 200-1000ppm, more preferably 300-800ppm, and further preferably 400-700 ppm.
In addition, the spinning assembly in the step 1) is positioned in a spinning box body; the temperature of the spinning manifold is 240-320 ℃, more preferably 250-310 ℃, further preferably 260-300 ℃, and further preferably 270-290 ℃; the pressure of the spinning assembly of the spinning manifold is 10-25MPa, preferably 12-23MPa, and more preferably 15-19 MPa.
And 2) cooling, oiling, stretching, heat setting and winding the raw silk in the step 2), namely, carrying out post-treatment on the raw silk to obtain the parallel composite fiber.
Wherein the cooling is by cross-air blowing; the wind speed of the cross air blow is 0.6-1.3m/s, preferably 0.8-1.1 m/s; the air temperature of the cross air blow is 15-27 ℃, preferably 18-25 ℃, and more preferably 20-23 ℃; the moisture of the cross air blower is 60-80%, preferably 68-73%.
The stretching process is more than 2-stage stretching; the total stretching multiple of the stretching is 1.5-5.0; the stretching temperature is 50-150 ℃, preferably 70-120 ℃.
The temperature of the heat setting is 120-200 ℃, and preferably 140-180 ℃.
The winding speed is 2200-5500m/min, preferably 2500-5000m/min, and more preferably 3000-3500 m/min.
The parallel composite fiber is soft, has good hygroscopicity, simultaneously has three-dimensional curling and high elasticity performance, can be widely applied to the knitting and tatting fields, and can be particularly applied to civil aspects such as socks, underwear, shirts, sweaters, carpets, swimsuits, outdoor clothes, sofas, down jackets, suits, fillers, cases, sewing threads and the like.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the side-by-side composite fiber prepared by the invention is soft and good in moisture absorption, has three-dimensional crimping performance and high elastic performance, and can be widely applied to the field of knitting and tatting.
Secondly, the selected polyamide 5X resin is made by a biological method, is a green material, does not depend on petroleum resources, does not cause serious pollution to the environment, and can reduce the emission of carbon and reduce the generation of greenhouse effect.
And thirdly, the preparation method of the short fiber is simple and easy to operate, has low production cost and is suitable for industrial production.
Detailed Description
The detection method of the performance parameters related in the invention is as follows:
1) relative viscosity:
concentrated sulfuric acid method by Ubbelohde viscometer: the dried polyamide 5X chips or short fiber samples thereof were accurately weighed at 0.25. + -. 0.0002g, dissolved by adding 50mL of concentrated sulfuric acid (96 wt%), and the concentrated sulfuric acid flowing time t0 and the polyamide sample solution flowing time t were measured and recorded in a thermostatic water bath at 25 ℃.
Viscosity number calculation formula: relative viscosity t/t0
t-solution flow time;
t0-solvent flow time.
2) Intrinsic viscosity:
solvent: phenol-tetrachloroethane (1:1) according to GB/T14901993 fibre grade polyester chip analysis method. Intrinsic viscosity ((1+1.4(t/t0-1))0.5-1)/0.7c (unit dL/g), t is the flow-out time of the solution, t0 is the flow-out time of the solvent, and c is the solution concentration.
3) Breaking strength, elongation at break, modulus:
the determination of the breaking strength and the breaking elongation can refer to the 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. Modulus is the breaking strength corresponding to 1% elongation at break x 100.
4) 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.
5) Crimping Properties
According to GB/T6506-2001, synthetic fiber textured yarn crimp performance test method.
Crimp shrinkage ═ ((L1-L2)/L1) × 100%;
crimp modulus ((L1-L3)/L1) × 100%;
crimp stability ═ 100% (L4-L1)/(L1-L2)) ×;
l1: fiber length measured after the fiber was subjected to a tension of 0.2cN/dtex for 10 s; l2: fiber length measured after the fiber was subjected to a tension of 0.001cN/dtex for 10 min; l3: the fiber length measured after the fiber was subjected to a tension of 0.01cN/dtex for 10 s; l4: fiber length measured after the fiber was subjected to a tension of 1.0cN/dtex for 10 seconds;
6) Elastic recovery:
untreated filaments were measured using an electronic single yarn strength tester YG061 at an ambient temperature of 23 ℃ and a humidity of 65%. The sample holding distance was 250mm, the drawing speed was 500mm/min, and the constant elongation values were set to 5%, 10%, and 15% of the holding gauge, respectively.
The treated filaments (100 ℃ for 15min) were treated with a fiber electron tester LLY06 at an ambient temperature of 23 ℃ and a humidity of 65%, the sample holding distance was 30mm, the drawing speed was 60mm/min, and the fixed elongation values were 50%, 100%, and 150% of the holding distance, respectively.
Elastic recovery rate ((L-L)1)/(L-L0) 100%) x in the formula: l is0The original length of the sample is obtained; l is the length of the sample after being stretched to a fixed extension; l is1The length of the sample after reset.
Example 1
1) Converging the polyamide 56 melt and the polyethylene glycol terephthalate melt in a composite spinning assembly through respective melt pipelines, and extruding through parallel composite spinneret plates to form primary yarns;
the proportion of the parallel composite components is accurately adjusted by a metering pump, the content of the polyamide 56 with the first parallel structure is 50 wt%, and the content of the polyethylene glycol terephthalate with the second parallel structure is 50 wt%.
The preparation method of the polyamide 56 melt comprises the following steps of heating polyamide 56 resin to a molten state in a screw extruder to form the melt, wherein the screw extruder is divided into five regions for heating: the temperature of the first zone is 245 ℃, the temperature of the second zone is 250 ℃, the temperature of the third zone is 265 ℃, the temperature of the fourth zone is 275 ℃, and the temperature of the fifth zone is 280 ℃; the polyamide 56 resin 96 wt% sulfuric acid has a relative viscosity of 2.8 and a water content of 300 ppm;
The polyethylene terephthalate melt is prepared by heating a polyethylene terephthalate resin to a molten state in a screw extruder, preferably divided into five zones, to form a melt: the temperature of the first zone is 255 ℃, the temperature of the second zone is 270 ℃, the temperature of the third zone is 285 ℃, the temperature of the fourth zone is 290 ℃ and the temperature of the fifth zone is 288 ℃; the intrinsic viscosity of the polyethylene terephthalate was 0.65dL/g, and the water content was 30 ppm.
The melt is extruded by a spinneret plate of a spinning manifold, the temperature of the spinning manifold is 285 ℃, and the pressure of a spinning assembly of the spinning manifold is 12 MPa.
2) Cooling, oiling, stretching, heat setting and winding the raw silk to obtain parallel composite fibers;
cooling by cross-blown air with the wind speed of 0.8m/s, the wind temperature of 26 ℃ and the humidity of the cross-blown air of 68 percent; the stretching process is 2-stage stretching, the total stretching multiple of the stretching is 2.5, the stretching temperature is 80 ℃, the heat setting temperature is 150 ℃, and the winding speed is 3500 m/min.
Example 2
1) Converging a polyamide 56 melt and a polytrimethylene terephthalate melt in a composite spinning assembly through respective melt pipelines, and extruding through parallel composite spinneret plates to form a primary yarn;
The proportion of the parallel composite components is accurately adjusted by a metering pump, the content of the polyamide 56 with the first parallel structure is 40 wt%, and the content of the polytrimethylene terephthalate with the second parallel structure is 60 wt%.
The preparation method of the polyamide 56 melt comprises the following steps of heating polyamide 56 resin to a molten state in a screw extruder to form the melt, wherein the screw extruder is divided into five regions for heating: the first zone temperature was 246 ℃; the temperature of the second zone is 258 ℃; the temperature of the three zones is 266 ℃; the temperature of the fourth zone is 278 ℃; the temperature of the fifth area is 285 ℃; the polyamide 56 resin 96 wt% sulfuric acid has a relative viscosity of 2.6 and a water content of 500 ppm;
the poly (trimethylene terephthalate) melt is prepared by heating poly (trimethylene terephthalate) resin to a molten state in a screw extruder, preferably divided into five zones, to form a melt: the temperature of the first zone is 257 ℃; the temperature of the second zone is 276 ℃; the temperature of the three zones is 283 ℃; the temperature of the fourth zone is 290 ℃; the temperature of the five zones is 284 ℃; the polytrimethylene terephthalate had an intrinsic viscosity of 1.0dL/g and a water content of 70 ppm.
The melt is extruded by a spinneret plate of a spinning manifold, the temperature of the spinning manifold is 284 ℃, and the pressure of a spinning assembly of the spinning manifold is 13 MPa.
2) Cooling, oiling, stretching, heat setting and winding the raw silk to obtain parallel composite fibers;
cooling by cross-blown air with the wind speed of 0.6m/s, the wind temperature of 24 ℃ and the humidity of the cross-blown air of 65 percent; the stretching process is 2-stage stretching, the total stretching multiple of the stretching is 2.8, the stretching temperature is 70 ℃, the heat setting temperature is 130 ℃, and the winding speed is 3800 m/min.
Example 3
1) Converging a polyamide 56 melt and a polybutylene terephthalate melt in a composite spinning assembly through respective melt pipelines, and extruding through parallel composite spinneret plates to form a primary yarn;
the proportion of the parallel composite components is accurately adjusted by a metering pump, the content of the polyamide 56 with the first parallel structure is 45 wt%, and the content of the polybutylene terephthalate with the second parallel structure is 55 wt%.
The melt of polyamide 56 is prepared by polymerizing pentanediamine and adipic acid to form polyamide 56. The method for preparing the polyamide 56 melt by directly polymerizing 1, 5-pentanediamine and adipic acid comprises the following steps: under the condition of nitrogen, 1, 5-pentanediamine, adipic acid and water are uniformly mixed to prepare a salt solution of polyamide 56; wherein the molar ratio of 1, 5-pentanediamine to adipic acid is 1.08: 1; then heating the salt solution of polyamide 56, raising the pressure in the reaction system to 2.2Mpa, exhausting, maintaining the pressure, reducing the pressure to reduce the pressure in the reaction system to gauge pressure of 0.1Mpa, and vacuumizing to the vacuum degree of-0.09 Mpa to obtain a polyamide 56 melt; in the reaction process, the temperature of the reaction system is 273 ℃ after pressure maintaining, 280 ℃ after pressure reduction and 273 ℃ after vacuum pumping. The polybutylene terephthalate melt is prepared by heating polybutylene terephthalate resin to a molten state in a screw extruder, which is preferably divided into five zones for heating: the temperature of the first zone is 255 ℃; the temperature of the second zone is 275 ℃; the temperature of the three zones is 285 ℃; the temperature of the fourth zone is 295 ℃; the temperature of the fifth zone is 290 ℃; the polybutylene terephthalate had an intrinsic viscosity of 0.8dL/g and a water content of 90 ppm.
The melt is extruded by a spinneret plate of a spinning manifold, the temperature of the spinning manifold is 290 ℃, and the pressure of a spinning assembly of the spinning manifold is 15 MPa.
2) Cooling, oiling, stretching, heat setting and winding the primary raw silk to obtain parallel composite fibers;
cooling by cross-blown air, wherein the air speed is 0.5m/s, the air temperature is 27 ℃, and the humidity of the cross-blown air is 67%; the stretching process is 2-stage stretching, the total stretching multiple of the stretching is 3.0, the stretching temperature is 78 ℃, the heat setting temperature is 140 ℃, and the winding speed is 4300 m/min.
Example 4
1) Converging the polyamide 56 melt and the polyamide 6 melt in a composite spinning assembly through respective melt pipelines, and extruding through parallel composite spinneret plates to form primary yarns;
the proportion of the parallel composite components is accurately adjusted by a metering pump, the content of the first parallel structure polyamide 56 is 35 wt%, and the content of the second parallel structure polyamide 6 is 65 wt%.
The preparation method of the polyamide 56 melt comprises the following steps of heating polyamide 56 resin to a molten state in a screw extruder to form the melt, wherein the screw extruder is divided into five regions for heating: the temperature of the first zone is 248 ℃; the temperature of the second zone is 262 ℃; the temperature of a third area is 275 ℃; the temperature of the fourth zone is 280 ℃; the temperature of the five zones is 275 ℃; the polyamide 56 resin 96 wt% sulfuric acid has a relative viscosity of 2.5 and a water content of 1000 ppm;
The polyamide 6 melt is prepared by heating the polyamide 6 resin to a molten state in a screw extruder, preferably divided into five zones, to form a melt: the temperature of the first zone is 250 ℃; the temperature of the second zone is 270 ℃; the temperature of the three zones is 280 ℃; the temperature of the fourth zone is 275 ℃; the temperature of the fifth area is 270 ℃; the polyamide 6 resin had a relative viscosity of 2.7 in 96 wt% sulfuric acid and a water content of 800 ppm.
The melt is extruded by a spinneret plate of a spinning manifold, the temperature of the spinning manifold is 270 ℃, and the pressure of a spinning assembly of the spinning manifold is 14 MPa.
2) Cooling, oiling, stretching, heat setting and winding the raw silk to obtain parallel composite fibers;
cooling by cross-blown air, wherein the air speed is 0.9m/s, the air temperature is 26 ℃, and the humidity of the cross-blown air is 72 percent; the stretching process is 2-stage stretching, the total stretching multiple of the stretching is 2.5, the stretching temperature is 60 ℃, the heat setting temperature is 160 ℃, and the winding speed is 4200 m/min.
Example 5
1) Converging the polyamide 56 melt and the polyamide 66 melt in a composite spinning assembly through respective melt pipelines, and extruding through parallel composite spinneret plates to form primary yarns;
the proportion of the parallel composite components is accurately adjusted by a metering pump, the content of the polyamide 56 with the first parallel structure is 50 wt%, and the content of the polybutylene terephthalate with the second parallel structure is 50 wt%.
The melt of polyamide 56 is prepared by polymerizing pentamethylene diamine and adipic acid to form polyamide 56.
The preparation method comprises the following steps: under the condition of nitrogen, 1, 5-pentanediamine, adipic acid, caprolactam and water are uniformly mixed to prepare a salt solution of polyamide 56, and meanwhile, a fluorescent whitening agent is added; wherein the molar ratio of the 1, 5-pentanediamine to the adipic acid is 1.06: 1, wherein the fluorescent whitening agent accounts for 1.2 wt% of the salt solution, and the caprolactam accounts for 1 wt% of the salt solution; then heating the salt solution of polyamide 56, raising the pressure in the reaction system to 2.2Mpa, exhausting, maintaining the pressure, reducing the pressure to reduce the pressure in the reaction system to gauge pressure of 0.3Mpa, and vacuumizing to-0.01 Mpa to obtain polyamide 56 melt; in the reaction process, the temperature of the reaction system is 277 ℃ after the pressure maintaining is finished, 282 ℃ after the pressure reducing is finished, and 278 ℃ after the vacuum pumping is carried out.
The polyamide 66 melt is prepared by heating the polyamide 66 resin to a molten state in a screw extruder, preferably divided into five zones for heating: the temperature of the first zone is 255 ℃; the temperature of the second zone is 275 ℃; the temperature of the three areas is 285 ℃; the temperature of the fourth zone is 295 ℃; the temperature of the fifth zone is 290 ℃; the polyamide 66 resin had a relative viscosity of 2.4 in 96 wt% sulfuric acid and a water content of 900 ppm.
The melt is extruded by a spinneret plate of a spinning manifold, the temperature of the spinning manifold is 290 ℃, and the pressure of a spinning assembly of the spinning manifold is 16 MPa.
2) Cooling, oiling, stretching, heat setting and winding the primary raw silk to obtain parallel composite fibers;
cooling by cross air blow with the air speed of 0.7m/s, the air temperature of 23 ℃ and the humidity of the cross air blow of 75%; the stretching process is 2-stage stretching, the total stretching multiple of the stretching is 2.8, the stretching temperature is 70 ℃, the heat setting temperature is 180 ℃, and the winding speed is 4500 m/min.
Example 6
1) Converging the polyamide 510 melt and the polytrimethylene terephthalate melt in a composite spinning assembly through respective melt pipelines, and extruding through parallel composite spinneret plates to form primary yarns;
the proportion of the parallel composite components is accurately adjusted by a metering pump, the content of the first parallel structure polyamide 510 is 40 wt%, and the content of the second parallel structure polytrimethylene terephthalate is 60 wt%.
The preparation method of the polyamide 510 melt comprises the following steps of heating polyamide 510 resin to a molten state in a screw extruder to form the melt, wherein the screw extruder is divided into five regions for heating: the temperature of the first zone is 240 ℃; the temperature of the second zone is 250 ℃; the temperature of the three zones is 260 ℃; the temperature of the fourth zone is 270 ℃; the temperature of the fifth zone is 280 ℃; the polyamide 510 resin 96 wt% sulfuric acid has a relative viscosity of 2.5 and a water content of 600 ppm;
The polypropylene terephthalate melt is prepared by heating a polypropylene terephthalate resin to a molten state in a screw extruder, preferably divided into five zones, to form a melt: the temperature of the first zone is 255 ℃; the temperature of the second zone is 265 ℃; the temperature of the three zones is 275 ℃; the temperature of the fourth zone is 285 ℃; the temperature of the fifth zone is 280 ℃; the intrinsic viscosity of the polypropylene terephthalate resin was 0.95dL/g, and the water content was 50 ppm.
The melt is extruded by a spinneret plate of a spinning manifold, the temperature of the spinning manifold is 280 ℃, and the pressure of a spinning assembly of the spinning manifold is 13 MPa.
2) Cooling, oiling, stretching, heat setting and winding the raw silk to obtain parallel composite fibers;
cooling by cross-blown air with the wind speed of 0.5m/s, the wind temperature of 28 ℃ and the humidity of the cross-blown air of 65 percent; the stretching process is 2-stage stretching, the total stretching multiple of the stretching is 3.0, the stretching temperature is 75 ℃, the heat setting temperature is 160 ℃, and the winding speed is 3200 m/min.
Example 7
1) Converging the polyamide 512 melt and the polyamide 6 melt in a composite spinning assembly through respective melt pipelines, and extruding through parallel composite spinneret plates to form primary yarns;
the proportion of the parallel composite components is accurately adjusted by a metering pump, the content of the first parallel structure polyamide 512 is 50 wt%, and the content of the second parallel structure polyamide 6 is 50 wt%.
The preparation method of the polyamide 512 melt comprises the following steps of heating polyamide 512 resin to a molten state in a screw extruder to form the melt, wherein the screw extruder is divided into five regions for heating: the temperature of the first zone is 242 ℃; the temperature of the second zone is 258 ℃; the temperature of the three zones is 268 ℃; the temperature of the fourth zone is 276 ℃; the temperature of the fifth area is 270 ℃; the polyamide 512 resin 96 wt% sulfuric acid has a relative viscosity of 2.5 and a water content of 600 ppm;
the polyamide 6 melt is prepared by heating the polyamide 6 resin to a molten state in a screw extruder, preferably divided into five zones, to form a melt: the temperature of the first zone is 250 ℃; the temperature of the second zone is 260 ℃; the temperature of a third area is 270 ℃; the temperature of the fourth zone is 282 ℃; the temperature of the five zones was 275 ℃.
The melt is extruded by a spinneret plate of a spinning manifold, the temperature of the spinning manifold is 270 ℃, and the pressure of a spinning assembly of the spinning manifold is 11 MPa.
2) Cooling, oiling, stretching, heat setting and winding the raw silk to obtain parallel composite fibers;
cooling by cross-blown air with the wind speed of 0.7m/s, the wind temperature of 25 ℃ and the humidity of the cross-blown air of 68 percent; the stretching process is 2-stage stretching, the total stretching multiple of the stretching is 2.5, the stretching temperature is 65 ℃, the heat setting temperature is 170 ℃, and the winding speed is 4800 m/min.
Comparative example 1
1) Converging the polyethylene terephthalate melt and the polytrimethylene terephthalate melt in a composite spinning assembly through respective melt pipelines, and extruding through parallel composite spinneret plates to form primary yarns;
the proportion of the parallel composite components is accurately adjusted by a metering pump, the content of the polyethylene glycol terephthalate with the first parallel structure is 50 wt%, and the content of the polytrimethylene terephthalate with the second parallel structure is 50 wt%.
The preparation method of the polyethylene terephthalate melt comprises the following steps of heating polyethylene terephthalate resin to a molten state in a screw extruder to form the melt, wherein the screw extruder is divided into five regions for heating: the first zone temperature was 244 ℃; the temperature of the second zone is 266 ℃; the temperature of the three zones is 278 ℃; the temperature of the fourth zone is 286 ℃; the temperature of the fifth zone is 290 ℃; the intrinsic viscosity of the polyethylene terephthalate is 0.67dL/g, and the water content is 50 ppm;
the polytrimethylene terephthalate melt is prepared by heating a polytrimethylene terephthalate resin to a molten state in a screw extruder, which is preferably divided into five zones for heating: the temperature of the first zone is 255 ℃; the temperature of the second zone is 270 ℃; the temperature of the three zones is 280 ℃; the temperature of the fourth zone is 290 ℃; the temperature of the fifth area is 290 ℃; the polytrimethylene terephthalate had an intrinsic viscosity of 1.0dL/g and a water content of 80 ppm.
The melt is extruded by a spinneret plate of a spinning manifold, the temperature of the spinning manifold is 290 ℃, and the pressure of a spinning assembly of the spinning manifold is 13 MPa.
2) Cooling, oiling, stretching, heat setting and winding the raw silk to obtain parallel composite fibers;
cooling by cross air blow with the air speed of 0.6m/s, the air temperature of 28 ℃ and the humidity of 65 percent; the stretching process is 2-stage stretching, the total stretching multiple of the stretching is 3.0, the stretching temperature is 90 ℃, the heat setting temperature is 160 ℃, and the winding speed is 4500 m/min.
Comparative example 2
1) Converging the polyethylene terephthalate melt and the polybutylene terephthalate melt in a composite spinning assembly through respective melt pipelines, and extruding through parallel composite spinneret plates to form primary yarns;
the proportion of the parallel composite components is accurately adjusted by a metering pump, the content of the polyethylene glycol terephthalate with the first parallel structure is 50 wt%, and the content of the polybutylene terephthalate with the second parallel structure is 50 wt%.
The preparation method of the polyethylene terephthalate melt comprises the following steps of heating polyethylene terephthalate resin to a molten state in a screw extruder to form the melt, wherein the screw extruder is divided into five regions for heating: the temperature of the first zone is 250 ℃; the temperature of the second zone is 265 ℃; the temperature of a third area is 275 ℃; the temperature of the fourth zone is 285 ℃; the temperature of the fifth area is 295 ℃; the intrinsic viscosity of the polyethylene terephthalate is 0.65dL/g, and the water content is 40 ppm;
The polybutylene terephthalate melt is prepared by heating a polybutylene terephthalate resin to a molten state in a screw extruder, which is preferably divided into five zones for heating: the temperature of the first zone is 258 ℃; the temperature of the second zone is 273 ℃; the temperature of the three zones is 285 ℃; the temperature of the fourth zone is 290 ℃; the temperature of the fifth zone is 288 ℃; the polybutylene terephthalate had an intrinsic viscosity of 0.8dL/g and a water content of 70 ppm.
The melt is extruded by a spinneret plate of a spinning manifold, the temperature of the spinning manifold is 290 ℃, and the pressure of a spinning assembly of the spinning manifold is 13 MPa.
2) Cooling, oiling, stretching, heat setting and winding the raw silk to obtain parallel composite fibers;
cooling by cross-blown air with the wind speed of 0.7m/s, the wind temperature of 25 ℃ and the humidity of the cross-blown air of 60 percent; the stretching process is 2-stage stretching, the total stretching multiple of the stretching is 2.0, the stretching temperature is 80 ℃, the heat setting temperature is 150 ℃, and the winding speed is 3300 m/min.
TABLE 1 fiber Properties in examples and comparative examples
TABLE 2 fiber Properties in examples and comparative examples